Fusion Engineering and Design 145 (2019) 46–53

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Fusion Engineering and Design

journal homepage: www.elsevier.com/locate/fusengdes

Microstructural and magnetic characteristics of ceramic dispersion T

strengthened sintered stainless steels after thermal ageing
⁎
Csaba Balázsia, , Haroune Rachid Ben Zinea,b, Monika Furkoa, Zsolt Czigánya, László Almásyc,
Vasyl Ryukhtind, Hiroaki Murakamie, Gültekin Göllerf, Onuralp Yucelf, Filiz Cinar Sahinf,
Katalin Balázsia, Satoru Kobayashie, Ákos Horvátha
a
Centre for Energy Research, Hungarian Academy of Sciences, Konkoly-Thege M. str. 29-33, 1121, Budapest, Hungary
b
Doctoral School of Materials Science and Technologies, Óbuda University, Bécsi str. 96/B, Budapest, Hungary
c
Wigner Research Centre for Physics, Hungarian Academy of Sciences, Konkoly-Thege M. str. 29-33, 1121, Budapest, Hungary
d
Nuclear Physics Institute, ASCR, Husinec - Řež 130, 250 68 Řež, Czech Republic
e
Iwate University, Faculty of Science andEngineering, Iwate University, 4-3-5 Ueda, Morioka, 020-8551, Japan
f
Istanbul Technical University, Metallurgical and Materials Engineering Deptartment, Maslak, 34469, Istanbul, Turkey

A R T I C LE I N FO A B S T R A C T

Keywords: The effect of the ultrafine grained silicon nitride and yttria addition to the morphological, structural, mechanical
Ceramic dispersion strengthened steels and magnetic properties of the ceramic dispersion strengthened 316 L stainless steels prepared by powder
Microstructure technology has been studied. Four composites have been prepared: 316 L/0.33 wt.% Si3N4, 316 L/1 wt.% Si3N4
Hardness (CDS) and 316 L/0.33 wt.% Y2O3, 316 L/1 wt.% Y2O3 (ODS). Spark plasma sintering (SPS) was used for fast
EBSD
compaction of milled composite powders. The hardness values have been found to be significantly higher in the
Magnetic properties
cases of CDS and ODS samples in comparison to reference sample, whereas the ODS composites had lower
smaller hardness than the CDS composites regardless the content of additives. The magnetic characterization of
samples demonstrated that the samples exhibit ferromagnetic property already before ageing and a larger fer-
romagnetic component was observed as a result of thermal aging. It was proven that in the case of ODS and CDS
samples with a low amount of Y2O3 or Si3N4 the saturation magnetization was slightly dependent on ageing
time, however, it exhibited a noticeable change with ageing both at 600 and 800 °C for samples containing
higher amount of additives.

1. Introduction Pressing (HIP) is a commonly used method to consolidate the ODS

Oxide dispersion strengthened (ODS) ferritic steels can be used as
large scale structural materials in many industrial applications owing to
their excellent corrosion resistance in oxidising and/or sulphidising
environments [1]. The ODS are useful base materials for boilers and
turbines of power generation plant co-firing coal or gas with renewable
fuels such as biomass for high temperature, high pressure tubing ap-
plications, fast breeder reactors and blanket applications for fusion re-
actors [2]. The ODS steels that exhibit remarkable irradiation swelling
resistance and excellent tensile, creep strength can easily be prepared
by powder metallurgy and they have ultra fine grained nanostructure
[3,4]. The superior performance of ODS ferritic steels over their con-
ventional heat resistance steels and austenitic steels is due to the high
density of nano-sized oxides within the matrix [5]. Powder metallurgy
is the main manufacture process of ODS steels [6]. Hot Isostatic
steels for controlling the microstructures and mechanical properties of
ODS steels. However, this process requires several hours exposure at
high temperatures over 1000 °C, so abnormal grain growth and pre-
cipitation coarsening can often be observed [7]. Compared to HIP,
Spark Plasma Sintering (SPS) is a novel powder consolidation tech-
nology. The main advantage of SPS is that it needs much less time in
both heating and cooling during sintering process. Moreover, SPS has
the ability to heat up the materials very quickly, providing a powerful
tool to retain the original nano-grains. Recently SPS has been employed
to prepare ODS steels [8]. The chemical composition of ODS is a crucial
point to the end-properties of ceramic dispersion strengthened 316 L/
Y2O3 composites [9]. The milling efficiency can be improved by adding
Y2O3 to the austenitic 316 L stainless steel powder; Y2O3 addition to the
composite matrix increased the hardness of the 316 L steel and sig-
nificantly reduced the wear rate [9].

⁎
Corresponding author.
E-mail address: balazsi.csaba@energia.mta.hu (C. Balázsi).

https://doi.org/10.1016/j.fusengdes.2019.05.035
Received 6 April 2019; Received in revised form 11 May 2019; Accepted 23 May 2019
Available online 27 May 2019
0920-3796/ © 2019 Published by Elsevier B.V.
C. Balázsi, et al.
Balázsi et al. [10] manufactured and investigated the structure of
two different nanostructured ODS steels. The initial steel powders were
prepared by dry and combined (dry and wet) milling. They investigated
the effect of the milling parameters on the microstucture, bending
strength and brittle behavior and found that the combined milling as-
sured higher strength and hardness compared to dry milling both in
austenitic and martensitic ODS samples. Austenitic and martensitic ODS
samples were also compared and it was found that combined milling
with consecutive SPS sintering was more efficient in the case of the
austenitic steel as more severe plastic deformation was observed in it. In
addition, microhardness measurements proved, that martensitic ODS is
twice as hard as the austenitic ODS [10]. This research group also in-
vestigated the effect of the submicrometer-sized Si3N4 addition on the
morphological and structural properties of the Si3N4/316 L stainless
steels composite. They found that the milling was not so effective in the
case of higher ceramic addition as almost globular 316 L stainless steel
grains with 50–100 μm in diameter were observed in ceramic dispersion
strenghtened steels (CDS) samples. The morphological investigations on
fractured surfaces of the sintered samples revealed the dominance of
the transgranular fracturing behavior in the 316 L/0.33 wt. % Si3N4
samples. However, in the 316 L/1 wt. % Si3N4 the SEM images showed
the dominance of the intergranular fracturing with the presence of very
few transgranular fracturing [11]. There are research works on in-
vestigation of the effect of different additives or reinforcements such as
carbon nanotube [12] and boron nitride (BN) [13], Si3N4 [14], TieYeO
[15] and TiC [16] on the phase composition, microstructure and me-
chanical properties of 316 L stainless steel consolidated by spark plasma
sintering. Staltsov et al. [17] produced more than 140 ferritic/mar-
tensitic reactor steel EP-450 samples to optimize the parameters of
mechanical alloying and spark-plasma sintering. They applied different
combination of time, speed of attritor rotation, pressure and con-
centration of strengthening particles to optimise the method for the
fabrication of ODS EP-450 steel with minimum porosity and maximum
density.
Boulnat et al. [18] manufactured a mechanically alloyed ferritic
ODS steel to investigate the grain growth, precipitation state in the
alloy and the appearance of heterogeneous grain structure. In their
work the base powder for high-chromium ferritic steels was produced
by gas atomization, while the ferritic powder was milled with yttria
particles (D < 100 nm), using an industrial high-energy attritor. They
used the SPS method to obtain different microstructures during the
consolidation process and described how the grain structure and the
precipitation state evolve and influence each other.
Guan et al. [19] developed 21-4 N austenitic stainless steel (ASS)
and 21-4 N ODS steel using mechanical alloying. The alloyed powders
were hot-pressed using 50 MPa at 1200 °C. Subsequently, the hot-
pressed samples were solution-treated and aged. They studied the
Vickers micro-hardness of the hot-pressed, solution- treated, and age-
treated ASS and ODS steels. The hot-pressed 21-4 N ASS and 21-4 N
ODS steels showed higher hardness than the solution-treated and aged
stainless steels. Hot-pressed 21-4 N ASS was found to have a hardness
value from 336 to 345 HV1.0, whereas 21-4 N ODS steel was found to
be 349–356 HV1.0. The microstructure of hot-pressed stainless steels
consisted of grain boundary carbides due to lower cooling rates. They
also reported that the solution treatment at 1150 °C eliminated the
grain boundary carbides in the hot-pressed steels and reduced the
hardness due to the dissolution. The ageing treatment at 750 °C in-
creased the hardness both in ASS and ODS steels by forming sufficient
amount of grain boundary carbides. Bartolomeu et al. [20] compared
three methods (selective laser melting (SLM), hot pressing and con-
ventional casting) and analysed the effect of the processing technolo-
gies on the microstructure, mechanical and wear behaviour of an aus-
tenitic 316 L stainless steel. The highest tensile strength, yield strength
and hardness were obtained for 316 L SS samples produced by selective
laser melting, while the 316 L SS samples produced by SLM technology
showed the greatest wear resistance. These improved properties were
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Fusion Engineering and Design 145 (2019) 46–53
attributed to the finer microstructure, induced by the selective laser
melting process. It was concluded that SLM technology is a good choice
to produce complex 316 L SS parts and fabricate customized body im-
plants with improved mechanical and wear performance.
In our research work we prepared ultrafine grained silicon nitride
and yttria added ceramic dispersion strengthened (CDS or ODS) 316 L
stainless steels by powder technology. The morphological, structural,
mechanical and magnetic properties of the ODS and CDS samples has
been thoroughly studied. The milled composite samples have been
compacted by spark plasma sintering (SPS) method. The structure of
CDS and ODS steels after thermal ageing has been evaluated with
magnetic measurements, electron back-scatter diffraction (EBSD), small
angle neutron scattering (SANS) and transmission electron microscopy
(TEM).
2. Experimental methods
2.1. Sample preparation
The austenitic 316 L stainless steel powder from Höganäs with
16.8Cr–12Ni–2.5Mo–1.5Mn – 0.6Si elemental composition and with
average grain size ˜70 μm and the Y2O3 powder grade C from H.C.
Starck with ˜700 nm in average particle size have been used to prepare
two composites: 316 L/0.33 wt% Y2O3 and 316 L/1 wt% Y2O3. In the
case of 316 L/0.33 wt% Si3N4 and 316 L/1 wt% Si3N4 the average grain
size of polygonal starting α-Si3N4 powder from UBE company was
around 300–400 nm. Attritor mill (Union Process 01-HD/HDDM) has
been used to decrease the grain size of steel and for homogeneous
distribution of the ceramic particles in the matrix. The composite
powders have been milled in ethanol media for 5 h at 600 rpm using
3 mm stainless steel balls with ball/material weight ratio of 10:1. The
composites have been sintered under 50 MPa mechanical pressure at
900 °C for 5 min dwelling time in vacuum using the Sinter-SPS-7.40MK-
VII apparatus in Istanbul Technical University. The diameter of sintered
discs was 100 mm and their thickness was around 9 mm. More details
about sample preparation can be found in our previous works [9–11].
The sintered samples have been investigated by mechanical testings
(HV, hardness), TEM, Keyence optical microscopy and small-angle
neutron scattering (SANS). Small pieces of ODS and CDS samples with
dimensions of 2 × 8 × 0.1 mm3 were cut from thin plates with electric
discharge machine. The samples were then mechanically polished,
followed by electrochemical polishing in a solution consisting of 10%
nitric acid and 90% acetic acid. The samples were enclosed in a vacuum
quarz tube and then aged at 600 °C in a high-temperature furnace up to
10 h and 20 h. For ODS and CDS with 1 wt.% Y2O3 and Si3N4, respec-
tively, ageing was carried out also at 800 °C. The detailed sample
parameters are summarized in Table 1.
2.2. Morphological characterization and surface roughness
Transmission Electron Microscopy (TEM, Philips CM-20 with
200 kV acceleration voltage) was used for structural and morphological
investigations of the structure and morphology of sintered samples. The
surface roughness was investigated by Keyence Microscope.
Table 1
Ageing parameters of samples.
Steel Additive content Ageing temperature Ageing time
wt.% °C h
ODS (Y2O3) 1.0 600, 800 0, 10, 20
0.33 600 0, 10, 20
CDS (Si3N4) 1 600, 800 0, 10, 20
0.33 600 0, 10, 20
C. Balázsi, et al.
2.3. Mechanical tests
The densities of composite discs were measured using Archimedes
method. The hardness of the sintered composites has been measured by
Vickers method where 5 N was applied for 10 s.
2.4. Small-angle neutron scattering (SANS) measurements
SANS measurements were performed at double-bent crystal SANS
instrument MAUD [21] (Neutron Physics Laboratory of Nuclear Physics
Institute in Řež). MAUD resolution covers a range of scattering vectors
(q) from 0.0002 to 0.002 nm−1 using thermal neutrons of wavelength
λ = 2.09 Å and a position sensitive gas detector. It permits to study
structural bulk inhomogenities sized from few tens of nm up to μm.
2.5. Magnetic and microstructural investigations after thermal treatment
Magnetic measurements were performed at room temperature with
superconducting quantum interference device (SQUID) magnetometer
(Quantum Design MPMS-5 L). Microstructures were evaluated with a
JEOL JSM-7001 F field-emission scanning electron microscope (FE-
SEM), equipped with Oxford Instruments electron-backscatter diffrac-
tion (EBSD) detector.
3. Results and discussion
3.1. Morphology of sintered composites
In Fig. 1, it is shown the surface morphology of sintered ODS (yttria
added) and TEM cross sections of CDS (silicon nitride added) samples.
In our previous works we thoroughly investigated and discussed the
morphology of milled powders prior to sintering process [9,11]. The
Fig. 1. TEM image of the sintered 316 L/0.33 wt.% Y2O3 composite (a), the sintered 316 L/1 wt.% Y2O3 composite (b), sintered 316 L/0.33 wt.% Si3N4 (c) and 316 L/
1 wt. % Si3N4 (d).
48
Fusion Engineering and Design 145 (2019) 46–53
results showed that the 5 h long wet milling changed the morphology of
both ODS and CDS samples containing different amount of ceramic
particles. The steel grains transformed from globular to lamellar shape
with average size of 40–100 μm. The added Y2O3 showed agglomera-
tion whereas Si3N4 particles were evenly distributed and covered the
surface of steel grains.
The results of roughness measurements taken on different samples
on the sintered and cut surfaces are demonstrated in Figs. 2 and 3. The
3D optical images and their evaluation revealed that the roughness of
samples is quite similar, it ranges between 20.4 and 23.1 μm. Ar-
ithmetical mean height (Sa) and maximum height (Sz) of samples are
also calculated and presented in Table 2. The Sa value is the extension
of Ra (arithmetical mean height of a line) to a surface. It expresses the
difference in height of each point compared to the arithmetical mean of
the surface. This parameter is used generally to evaluate surface
roughness, while the Sz value is defined as the sum of the largest peak
height value and the largest pit depth value within the defined area.
The 0.33 wt.% addition gave higher roughness values in both cases
(Table 2).
3.2. Mechanical measurements
The hardness and density values of different samples can be seen in
Fig. 4. It is visible, that the 316 L/Y2O3 composites (ODS) have slightly
higher densities compared to the 316 L/Si3N4 composites (CDS) pre-
pared by the same parameters [22], however their values hardly
changed with addition of 0.33 and 1 wt.% ceramic and oxide particles
into the matrix.
The CDS and ODS composites are all harder than the 316 L reference
sample as it is represented in Fig. 4. The HV values are significantly
higher in the cases of CDS and ODS samples than that for reference
sample. It is also visible that the ODS composites had a little smaller
C. Balázsi, et al. Fusion Engineering and Design 145 (2019) 46–53

Fig. 2. Roughness measurements on 316 L/0.33 wt.% Si3N4 composite (a, b) and on 316 L/1 wt.% Si3N4 (c, d). Magnification: 1000X.

Fig. 3. Roughness measurements on 316 L/0.33 wt.% Y2O3 composite (a, b) and on 316 L/1 wt.% Y2O3 (c, d). Magnification: 1000X.

hardness values than the CDS composites (where ultrafine ceramic
particles were more evenly distributed on the surface of steel grains)
regardless of the additive content. In our measurements, higher den-
sities of ODS composites were obtained than in the case of similar
composites made by the 3-Dimensional Fiber Deposition (3DFD) tech-
nique, even when higher sintering temperatures were applied [23].
3.3. Small-angle neutron scattering analysis
SANS data measured on the sintered samples at DBC-SANS facility
are presented in Fig. 5. The scattering curves on samples with Yttria
additions (Fig. 5a) obey Porod law (I˜Q−3) over the whole measured q-
range. This corresponds to the interface scattering from particles larger
than several micrometers. Same scattering behaviour is observed for

49
C. Balázsi, et al.
Table 2
Area roughness parameters of sintered ODS and CDS samples.
Steel Additive content / wt.% Sa / μm Sz / μm
CDS (Si3N4) 0.33 2.8 22.2
1.0 2.6 20.6
ODS (Y2O3) 0.33 2.6 23.2
1 2.5 20.5
Fig. 4. Density (g/cm3) and hardness (GPa) values of CDS and ODS samples.
sample with 1 wt% of Si3N4 (Fig. 5b). However, SANS on 316 L
+0.33 wt% of Si3N4 has demonstrated presence of smaller (submicron)
size particles. The scattering data were fitted to a model scattering of
spherical particles with log-normal size distribution, and the fitted
averaged diameter is obtained as < D > = 441 ± 33 nm. The pre-
sence of smaller grains in this sample is probably caused by their better
dispersion in the steel matrix, and contribute to the favourable me-
chanical properties of these CDS (Fig. 4). Morphological investigations
of milled powders and sintered composites have also been studied in
our earlier works [9,11]. It was observed that the 5 h wet milling in-
duced striking morphological changes of 316 L/ 0.33 wt. % Si3N4 grains
of powders mixtures. The steel grains transformed from a globular to
lamellar shape with two typical average sizes, 100 μm and 40 μm. The
Si3N4 addition was distributed homogeneously and covered the surface
of steel grains, this polydispersed tendency of small ceramic particles
was demonstrated here by SANS again (Fig. 5b).
As can be concluded by analysing of the SANS data, the specimen of
1 wt. % Si3N4, 0.33 wt% Y2O3 and 1 wt% Y2O3 addition the milling was
not as effective as in the case of 0.33 wt. % Si3N4 addition. In those
cases the SANS results show higher grain sizes for ceramic particle
additions. The Porod law demonstrates the smooth ceramic-steel in-
terfaces at the studied magnifications ˜ 100 nm.
Fig. 5. SANS scattering curves of CDS and ODS samples with Y2O3 (a) and Si3N4 (b) ceramic additions.
50
Fusion Engineering and Design 145 (2019) 46–53
3.4. Magnetic and microstructural investigations after thermal treatment
Fig. 6(a) and (b) shows magnetization curves for ODS samples with
1.0 wt.% Y2O3, aged at 600 and 800 °C up to 20 h, respectively. Mag-
netization exhibits almost linear behavior with field before and after
ageing for both samples and its slope seems to slighly become larger
after ageing, indicating a slight increase of magnetic susceptibility
during ageing. This behavior was also observed for ODS samples with
0.33 wt.% Y2O3 aged at 600 °C (not shown).
Fig. 6(c) and (d) shows data for CDS samples with 1.0 wt.% Si3N4
inclusion, aged at 600 and 800 °C, respectively. Both samples exhibit
ferromagnetic property before ageing, associated with a hysteresis
around zero magnetic field. In particular, for the sample used for ageing
at 800 °C, we observed a large ferromagnetic component, which evolves
with thermal ageing. Considering that both samples used for ageing at
600 °C and 800 °C were cut from the identical plate, a ferromagnetic
phase is present inhomogeneously for 1.0 wt.% Si3N4 CDS samples.
Fig. 7(a) and 7(b) summarize saturation magnetization as a function
of ageing time for ODS and CDS samples, respectively. Saturation
magnetization was determined by extrapolating high-field magnetiza-
tion data to zero field. It was observed that the ODS and CDS samples
with a low amount of Y2O3 or Si3N4, the saturation magnetization was
very weakly dependent on ageing time, it exhibited a noticeable change
with ageing both at 600 and 800 °C for samples containing higher
amount of additives.
To investigate possible microstructural changes with ageing, EBSD
measurements were performed for ODS and CDS samples with 1.0 wt.%
Y2O3 and Si3N4, respectively, aged at 800 °C. Fig. 8 shows EBSD inverse
pole figure (IPF) map and phase color map for ODS sample before and
after ageing at 20 h. The IPF map shows that the sample contains grains
with variable size ranging from a few micron to a hundred micron. The
average grain size is approximately 11 μm and it did not show any
noticeable change with ageing. The phase color map indicates that the
sample contains approximately > 90% austenitic phase with fcc struc-
ture, and the phase is stable even after ageing at 800 °C up to 20 h. No
bcc iron was detected in the investigated area shown in Fig. 8. How-
ever, in the other area of the sample, a very small amount of bcc iron
structure (< ˜0.2%) was detected; this amount changes depending on
the investigated area.
Similar results were obtained also for CDS sample with 1.0 wt.%
Si3N4 shown in Fig. 8. The average grain size is ˜14 μm and small
amount of bcc iron structure (< ˜0.2%) was also detected for this
sample. No pronounced ageing effect on microstructure was observed
and experimental evidence showing an increase of volume fraction of
bcc iron which may contribute to an increase of saturation magneti-
zation shown in Fig. 7 was not obtained from the present EBSD mea-
surements. Detailed microstructural observations with EBSD are in
progress to understand magnetic property changes during ageing
(Fig. 9).
C. Balázsi, et al. Fusion Engineering and Design 145 (2019) 46–53

Fig. 6. Magnetization curves for 1.0 wt.% Y2O3 ODS samples aged at (a) 600 °C and (b) 800 °C, and for 1.0 wt.% Si3N4 CDS samples aged at (c) 600 °C and (d) 800 °C.
Inset in (c) shows an enlargement of the data around zero field.

Fig. 7. Saturation magnetization Ms as a function ageing time for (a) ODS and (b) CDS samples. The inset in (b) shows the enlargement around low Ms.

4. Conclusion
Four composites were prepared: 316 L/0.33 wt.% Si3N4, 316 L/1 wt.
% Si3N4 and 316 L/0.33 wt.% Y2O3, 316 L/1 wt.% Y2O3 by spark
plasma sintering (SPS). The optimal coverage of 316 L stainless steel
grains with ceramic submicrometer-sized particles was obtained by
intensive milling. The added Y2O3 and Si3N4 particles were evenly
distributed and covered the surface of steel grains. The evaluation of
roughness measurements revealed that the roughness of all samples is
quite similar, it ranged between 20.4 and 23.1 μm. The hardness values
were significantly higher in the cases of CDS and ODS samples than that
for reference sample and the ODS composites had a little smaller
hardness than the CDS composites regardless the content of additives.
The submicron sized particles were detected by SANS in CDS with lower
concentration (0.33 wt%) of Si3N4 additives, whereas other composi-
tions contain structures larger than several micrometers. The magnetic
characterization of samples demonstrated that the samples exhibit
ferromagnetic property before ageing and a large ferromagnetic com-
ponent was observed, which evolved with thermal aging. It was proven
that for ODS and CDS samples with a low amount of Y2O3 or Si3N4, the
saturation magnetization was slightly dependent on ageing time,
however, it exhibited a noticeable change with ageing both at 600 and
800 °C for samples containing higher amount of additives.

51
C. Balázsi, et al.
Fig. 9. EBSD inverse pole figure (IPF) map of CDS samples with 1.0 wt.% Si3N4 for ageing time of 0 (a) and 20 h (b), showing crystal orientation along the normal
direction of sample surface. The insets show phase color map. The crystal structure of Si3N4 was not considered in this analysis.
Acknowledgements
The support of Hungarian-Japanese project "Development of elec-
tromagnetic non-destructive evaluation method for aging degradation
of chromium steels at high temperatures” financed by Hungarian
Academy of Sciences (HAS) and Japan Society for the Promotion of
Science (JSPS) is highly acknowledged. Mr. Haroune Rachid Ben Zine
thanks to Hungaricum Stipendium and MTA EK project “Nanostructural
ODS steel development” for support. Thanks to COST Action CA15102
Solutions for Critical Raw Materials under Extreme Conditions support.
SANS measurements were carried out at the CANAM infrastructure
through MŠMT project No. LM2015056 and infrastructure of Reactors
LVR-15 and LR-0, which is financially supported by project
LM2015074.
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