N u c l e a r E n g i n e e r i n g a n d T e c h n o l o g y 4 9 ( 2 0 1 7 ) 1 7 8 e1 8 8

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Nuclear Engineering and Technology

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Original Article

Microstructure Refinement and Strengthening

Mechanisms of a 9Cr Oxide Dispersion
Strengthened Steel by Zirconium Addition

Haijian Xu a,b, Zheng Lu a,*, Dongmei Wang a, and Chunming Liu a

a
Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and
Engineering, Northeastern University, 3-11 Wenhua Road, Shenyang 110819, China
b
Material Science and Engineering, Graduate School of Engineering, Hokkaido University, N20, W15, Chuou-ku,
Sapporo 060-8628, Japan

article info abstract

Article history: To study the effects of zirconium (Zr) addition on the microstructure, hardness and the
Received 10 March 2016 tensile properties of oxide dispersion strengthened (ODS) ferriticemartensitic steels, two
Received in revised form kinds of 9Cr-ODS ferriticemartensitic steels with nominal compositions (wt.%) of Fe-9Cr-
24 August 2016 2W-0.3Y2O3 and Fe-9Cr-2W-0.3Zr-0.3Y2O3 were fabricated by the mechanical alloying (MA)
Accepted 9 September 2016 of premixed powders and then consolidated by hot isostatic pressing (HIP) techniques. The
Available online 16 January 2017 experimental results showed that the average grain size decreases with Zr addition. The
trigonal d-phase Y4Zr3O12 oxides and body-centered cubic Y2O3 oxides are formed in the
9Cr-Zr-ODS steel and 9Cr non-Zr ODS steel, respectively, and the average size of Y4Zr3O12
Keywords: particles is much smaller than that of Y2O3. The dispersion morphology of the oxide par-
9Cr-ODS Steel ticles in 9Cr-Zr-ODS steel is significantly improved and the number density is 1.1
1023/m3
Hardness with Zr addition. The 9Cr-Zr-ODS steel shows much higher tensile ductility, ultimate
HIP tensile strength and Vickers hardness at the same time.
Microstructure Copyright © 2017, Published by Elsevier Korea LLC on behalf of Korean Nuclear Society. This
Tensile Property is an open access article under the CC BY-NC-ND license (http://creativecommons.org/
licenses/by-nc-nd/4.0/).

1. Introduction mechanical properties and significantly higher irradiation

resistance due to high-density nano-sized oxide particles,
Nano-structured oxide dispersion strengthened (ODS) ferri- which are effective barriers to pin dislocations and sinks for
ticemartensitic steels are the leadings candidates for point defects [4e8]. Fine, high density and stable oxide parti-
advanced sodium-cooled fast reactors and further fusion en- cles are the guarantee that ODS steels can be widely used in
ergy systems [1e3]. Compared to other conventional reduced energy systems. Yttria or yttrium oxide is commonly intro-
activation ferriticemartensitic steels, ODS ferri- duced to ODS steels. However the oxide particle size increases
ticemartensitic steels possess excellent high-temperature remarkably during the consolidation and heat treatment

* Corresponding author.
E-mail address: luz@atm.neu.edu.cn (Z. Lu).
http://dx.doi.org/10.1016/j.net.2017.01.002
1738-5733/Copyright © 2017, Published by Elsevier Korea LLC on behalf of Korean Nuclear Society. This is an open access article under
the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
 N u c l e a r E n g i n e e r i n g a n d T e c h n o l o g y 4 9 ( 2 0 1 7 ) 1 7 8 e1 8 8
process. It is important to control the oxide particle size and
density, hence titanium (Ti) is chosen for addition to ODS
steels [9]. Some previous investigations [10e13] found that
nano-Y-Ti-O particles were good for improving the high-
temperature properties of ODS steels. Some researchers re-
ported that Fe-Zr alloys which were produced by mechanical
alloying (MA), were resistant to grain growth even though the
annealing temperature reaches up to 1,373 C [14]. In ODS steel
containing aluminum, the addition of Zr elements refined the
oxide particles [15]. According to the first principle calculation
results, the binding energy of Y-Zr-O clusters was higher than
that of Y-Al-O and Y-Ti-O clusters in Fe matrix, which meaned
that the Y-Zr-O phase was easier to form and more stable
because the higher stability of these clusters might enhance
the nucleation rate and then decreased the size of these
clusters with Zr addition [16e19]. However, the influence of Zr
addition on the microstructure and mechanical properties of
9Cr-ODS ferriticemartensitic steels without Al addition has
not been substantially investigated. In this research, in order
to clarify the mechanism of oxide particle formation and to
study the effect of the Zr addition on the improvement of
particle characteristics and mechanical properties, two kinds
of 9Cr-ODS ferriticemartensitic steels with nominal compo-
sitions of Fe-9Cr-2W- 0.3Y2O3 and Fe-9Cr- 2W-0.3Zr-0.3Y2O3
were fabricated by MA and hot isostatic pressing (HIP). The
grain size, the structure of oxide particles, distribution of
oxide particles, and mechanical properties of the 9Cr-ODS
steels were characterized.
2. Materials and methods
The 9Cr-ODS steels with the nominal compositions of Fe-9Cr-
2W-0.3Y2O3 (wt.%, designated as 9Cr-non-Zr-ODS) and Fe-9Cr-
2W-0.3Zr-0.3Y2O3 (designated as 9Cr-Zr-ODS) were prepared
by MA, using high-purity metal powders of Fe, Cr, W, Zr, and
Y2O3 with purities of: 99.5 wt.%, 99 wt.%, 99.9 wt.%, 99.5 wt.%
and 99.99 wt.%, respectively. The compositions of two kinds of
ODS steels after HIP were measured by the inert gas pulse
infrared thermal conductivity method and is listed in Table 1.
MA was conducted in a FRITSCH Pulverisette5 planetary mill
for 48 hours with a rotation speed of 260 rpm and ball-to-
powder ratio of 10:1 under high-purity Ar atmosphere at
room temperature (RT). The MA powders were then degassed
and sealed into a mild steel can, followed by HIP at 1,100 C for
2 hours under a pressure of 200 MPa.
To investigate the effect of Zr addition on the grain size, the
electron backscatter diffraction (EBSD) specimens cut from
HIPed bars with dimensions 3
5
10 mm3 were examined on
a JEOL JSM7001F scanning electron microscope (SEM) after
electro-polishing in a step length of 0.1 mm/s. After surface
Table 1 e Actual chemical composition of the
investigated specimens (wt.%).
Alloy Cr W Zr Y C O Fe
9Cr-non-Zr 8.89 1.89 e 0.27 0.05 0.16
9Cr-Zr 9.05 1.95 0.33 0.26 0.05 0.17
Bal., balance.
179
grinding with silicon carbide papers, the specimens were
finally polished using a suspension of colloidal silica to
remove the mechanical distortion. The precipitates of the
specimens were investigated by transmission electron mi-
croscopy (TEM) using a JEM-2100F operated at 200 kV. Speci-
mens for TEM-high resolution transmission electron
microscopy (HRTEM) observation were mechanically thinned
to 50e60 mm and then electrochemically thinned with a so-
lution composed of HClO4 and CH3COOH (1:19) at 253 K in a
TENUPOL device. The crystal structures of the oxide particles
were analyzed by HRTEM with a double tilt specimen holder.
HRTEM images of the oxide particles were taken in the thin
regions near the TEM specimen edge and then evaluated by
means of fast Fourier transformation (FFT). When deter-
mining the number density of oxide particles, the local foil
thickness was measured by the converged-beam electron
diffraction method [20,21]. The tensile tests of flat specimens
1-mm thick, 3-mm wide, and 13-mm gauge length were pre-
pared from the HIPed bar. A tensile test was carried out on an
SANS-CMT5105 electro-mechanical machine at a constant
strain rate of 2
10e3 mm/s at RT (25 C) and 700 C, respec-
tively. The tests were performed three times at each
temperature.
Vickers microhardness tests were performed with the di-
mensions 3
5
10 mm3 by using a 401MVDTM Vickers
hardness tester at a load of 100 g. The hardness values were
determined based on the average of 10 points. The
morphology of the fracture surfaces of the tensile specimens
was investigated by SEM (JSM-6510A).
3. Results
3.1. Microstructural characterization
The microstructural characterizations for the 9Cr-non-Zr-
ODS steel and 9Cr-Zr-ODS steel by EBSD analyses are shown in
Figs. 1A and 1B. Fig. 1 shows the inverse pole figure of the 9Cr-
ODS specimens. The 9Cr-ODS steels exhibit fine and nearly
equiaxed grains, whether they contain Zr or not. No evident
anisotropies are observed in the microstructure and the
average grain sizes are about 1.2 mm and 0.8 mm, respectively.
The grain size of the specimen of the 9Cr-Zr-ODS steel, as
shown in Fig. 1B, is much smaller than that of the 9Cr-non-Zr-
ODS steel in Fig. 1A. It indicates that an addition of Zr leads to
the finer grain size.
Fig. 2 shows the TEM images of 9Cr-non-Zr-ODS steel and
9Cr-Zr-ODS steel. It is found that the average grain size of the
fabricated steels is very fine, in which the big grain diameter is
several microns and the small grain diameter is hundredths of
a nanometer. Oxide particles are dispersed inside the grains
and along the grain boundaries. It is evident that the grains of
the 9Cr-ODS steel are refined by Zr addition, which is in
accordance with the result of the EBSD result in Fig. 1.
The grain boundary maps corresponding to Fig. 1 are
shown in Fig. 3. The low angle boundary of 2e15 is decorated
with green lines and the high angle boundary is decorated
Bal.
with black lines. Fig. 4A shows that the histograms of the
Bal.
misorientation angles of 9Cr-ODS steels are similar to other
ODS steels and heat-resistant steel [22e24]. A maximum peak
180 N u c l e a r E n g i n e e r i n g a n d T e c h n o l o g y 4 9 ( 2 0 1 7 ) 1 7 8 e1 8 8
Fig. 1 e Inversed pole figures maps of 9Cr-ODS steels. (A) 9Cr-non-Zr ODS steel. (B) 9Cr-Zr-ODS steel. ODS, oxide dispersion
strengthened.
Fig. 2 e Transmission electron microscopy images of grain morphologies for 9Cr-ODS steels. (A) 9Cr-non-Zr-ODS steel. (B)
9Cr-Zr-ODS steel. ODS, oxide dispersion strengthened.
appears in the smallest angle, which illustrates that there is a
great quantity of the subgrain boundaries in accordance with
those found in boundary maps (Fig. 3). Another misorientation
peak appears around 60 , which may have some connection
with the twinning process during the formation of martensite
[25]. Fig. 4B shows that the misorientation angle distribution
does not change noticeably except for a minor increase in the
fraction of the lowest misorientation angles in the 9Cr-Zr-ODS
steel. Therefore, the oxide particle size decreases and the
number density increases with Zr addition as seen in section
3.2, which can more effectively pin dislocations and sub-
grain boundaries, and inhibit the subgrain recovery in the HIP
process.
3.2. Size distributions and crystal structures of oxide
particles
Fig. 5A and 5B show the bright field images of oxide particles in
the matrix of 9Cr-non-Zr ODS steel and 9Cr-Zr-ODS steel,
respectively. A high density of oxide particles with a size of <
45 nm can be observed in the TEM bright field in underfocused
images. This shows that almost all the oxide particles are
spherical with a diameter of 3e10 nm. Fig. 6 shows the size
distribution of the oxide particles obtained by a direct mea-
surement of 1,000 oxide particles on TEM images from each
specimen. It is found that the frequency distribution of finer
particles increases, affected by incorporating Zr which leads
to a decrease in the mean particle size. The oxide particles
with a diameter < 10 nm constitute 85% and 92% in the matrix
of 9Cr-non-Zr-ODS steel and 9Cr-Zr-ODS steel, respectively.
For the oxide particles in 9Cr-non-Zr-ODS steel and 9Cr-Zr-
ODS steel, the mean diameter and total number density are
6.8 nm, 6.2
1022/m3 and 4.75 nm, 1.1
1023/m3, respectively.
Phase identification of these small oxide particles (diam-
eter < 10 nm) was performed by HRTEM. According to the
statistical results of HRTEM analyses, in the 9Cr-non-Zr-ODS
steel, small particles (diameter < 10 nm), are consistent with
cubic structure Y2O3. Fig. 7 shows the lattice images of
different sizes of Y2O3 oxide particles and their FFT images.
The Y2O3 particles shown in Fig. 7 are oriented with [01-1]
zone axis to the electron beam. Table 2 shows the inter-
planar distances and angles of the oxide particles.
The large particles (diameter > 10 nm) in the grains of the
9Cr-non-Zr-ODS steel are mainly identified as monoclinic
YCrO3 oxide particles. Fig. 8 shows a lattice image of the YCrO3
oxide particle (diameter, 15 nm), its FFT image and FFT filtered
image, in which the two measured atomic plane distances are
2.62 Å and 3.77 Å, with an angle of 90 . This result is in good
agreement with the YCrO3. The monoclinic YCrO3 oxide par-
ticle is oriented with [-101] zone axis.
In 9Cr-Zr-ODS steel, the small particles (diameter, < 10 nm)
are trigonal d-phase Y4Zr3O12 oxide particles. No Y2O3 oxide
particles are identified. The formation of Y4Zr3O12 reveals the
occurrence of internal oxidation reactions 2Y2O3 þ 3ZrO2 -
¼ Y4Zr3O12 during consolidation due to the stronger interac-
tion between Y and Zr [18]. Fig. 9 shows the lattice image of
 N u c l e a r E n g i n e e r i n g a n d T e c h n o l o g y 4 9 ( 2 0 1 7 ) 1 7 8 e1 8 8 181

Fig. 3 e Grain boundary maps of 9Cr-ODS steels. (A) 9Cr-non-Zr-ODS steel. (B) 9Cr-Zr-ODS steel. ODS, oxide dispersion
strengthened.

Fig. 4 e Misorientation angles of 9Cr-ODS steels. (A) The dependence of grain boundary misorientation angle of 9Cr-ODS
steels. (B) Frequency of the grain angles between LAG and HAG of 9Cr-ODS steels. HAG, high angle grain; LAG, low angle
grain; ODS, oxide dispersion strengthened.

Y4Zr3O12 oxide particles (diameter, 4 nm), the FFT image, the
FFT filtered image and the stimulated diffraction pattern from
the [-210] zone axis. Two measured atomic plane distances are
3.038 Å and 3.008 Å, with an angle of 109 . This result is in good
agreement with the trigonal d-phase Y4Zr3O12. Fig. 9D shows
stimulated diffraction patterns from the [-210] zone axis,
which agrees well with the FFT image from Y4Zr3O12 in Fig. 9B.
Similar large particles (diameter > 10 nm) in the grains of the
9Cr-Zr-ODS steel were observed by HRTEM. The HRTEM
image, corresponding FFT image and FFT filtered image are
shown in Fig. 10, in which the two measured atomic plane
distances are 2.758 Å and 2.096 Å, with an angle of 117 . This
result is in good agreement with the YCrO3. The monoclinic
YCrO3 oxide particle is oriented with [3-23] zone axis to the
electron beam.
Uchida et al. [26] found that Zr addition led to finer oxides
due to the stronger interaction between Y, Zr, and O and their
cluster compared to Y, Ti, and O. As a result, Y-Zr-O oxide
particles can hinder strongly the grain growth. Darling et al.
[27] noticed that Zr in a solute state could also prevent grain
growth, and Zr solutes in Fe produced high elastic misfit strain
energy and then lowered the free energy of grain boundary in
nanocrystalline materials. So a constituent of Zr not only
contributes to the formation of oxide particles which are
dispersed inside the grains and along the grain boundaries but
it may also be in a solute state and hinder the grain growth,
which is in accordance with the result of the grain boundary
misorientation angle shown in Fig. 4.
3.3. Mechanical properties
The addition of Zr to the 9Cr-ODS steels modifies the size,
density, and structure of the oxide particles. In this regard, it
also affects the mechanical properties of ODS steels. The
hardness value of the 9Cr-non-Zr-ODS is 351 ± 9 HV and the
hardness increases to 436 ± 8 HV in the 9Cr-ODS steel with Zr
addition. The increase in the hardness value also contributes
to the increase in the number density of precipitates and the
decrease in the average grain size. Figs. 11 and 12 show the
tensile stressestrain curves of the ODS steels and average
values of tensile properties of two ODS steels at each tem-
perature. It is found that the ultimate tensile strength (UTS)
182 N u c l e a r E n g i n e e r i n g a n d T e c h n o l o g y 4 9 ( 2 0 1 7 ) 1 7 8 e1 8 8

Fig. 5 e Bright field images of oxide particles in the matrix of 9Cr-ODS steels. (A) 9Cr-non-Zr-ODS steel. (B) 9Cr-Zr-ODS steel.
ODS, oxide dispersion strengthened.

Fig. 6 e Size distribution of the oxide particles in the matrix of 9Cr-ODS steels. ODS, oxide dispersion strengthened.

and total elongation (TE) of the ODS steels increases with the
Zr addition. It can be seen that the UTS of the 9Cr-ODS steels
decreases and the TE increases with the increase of the
measuring temperature. The UTS of 9Cr-non-Zr-ODS steel
and 9Cr-Zr-ODS steel are 1,406 MPa, 231 MPa, 1,503 MPa, and
332 MPa, and the TE are 2.8%, 16.2%, 4.9%, and 18.1% at RT
and 700 C, respectively. The reasons for the enhanced me-
chanical properties can be attributed to three factors. Firstly,
according to the Orowan strengthening mechanism [28], with
the Zr addition, the average size of the oxide particles in the
ODS steel decreases markedly, whereas the number density
of the oxide particles increases. Compared to the 9Cr-non-Zr-
ODS steel in Fig. 5, the distance between neighboring oxide
particles are reduced in 9Cr-Zr-ODS steel, resulting in
enhanced strength. Secondly, Dou et al. [15] proved that
nano-sized Y4Zr3O12 oxide particles are coherent with the
matrix. The coherent interface between the Y4Zr3O12 oxide
particles and the matrix hinders the formation and propa-
gation of microcracks which can effectively pin dislocations.
Thirdly, Zr may tend to diffuse grain boundaries due to
 N u c l e a r E n g i n e e r i n g a n d T e c h n o l o g y 4 9 ( 2 0 1 7 ) 1 7 8 e1 8 8
Fig. 7 e Y2O3 oxide particles. (A) High resolution transmission electron micrograph of Y2O3 oxide particles in the 9Cr-non-Zr-
ODS steel. (B) Fast Fourier transformation diagram of the micrograph in (A). ODS, oxide dispersion strengthened.
higher binding energy with vacancies which contributes to
form oxide particles inside the grain and along the grain
boundary. Otherwise, the higher strength and ductility of Zr-
ODS steel compared to non-Zr-ODS steel can also be attrib-
uted to the finer grain size. It is well known that grain
refinement results in an increase in both strength and
ductility.
Fig. 13 shows the SEM fracture micrographs of non-Zr and
Zr-ODS steels after the tensile test. Except for cleavages in
fracture surface, as shown in Fig. 13A, the dimples are rarely
observed in the sample of non-Zr-ODS steel after the tensile
test at RT, which implies a brittle fracture feature. A similar
phenomenon is found in the sample of Zr-ODS steel where the
cleavages’ surface areas become small, as shown in Fig. 13B,
which is in accordance with the results of the microstructure
and mechanical properties.
3.4. Yield strength evaluation
The yield strength of ODS steel can be expressed as a combi-
nation of matrix strength and contributions from a variety of
strengthening mechanisms as follows: (1) solid solution
strengthening due to the addition of Cr, W and C (due to
contamination from the MA process); (2) the indirect
strengthening due to grain refinement (HallePetch relation-
ship); and (3) dispersion strengthening from oxide particles.
The yield strength (sys) of ODS steel at RT can be estimated by:
sys ¼ s0 þ sss þ sp þ sk, where s0 is the matrix strength, sk is the
contribution from grain size, sss is the contribution from solid
solution strengthening and sp is the contribution of nano-
sized oxide particles. The base matrix strength is the stress
needed to move dislocations without other obstacles and can
be represented as s0. For as-received material, this value is
Table 2 e Particle size, index, interplanar distances and
angles of particles.
Number Particle size (nm) (h1k1l1) (h2k2l2)
d1 (Å) d2 (Å)
1 3.1 (422) (4-4-4)
2.16 1.53
2 4.9 (222) (400)
3.06 (2.65)
183
close to the yield strength of the pure iron. A value of 125 MPa
was chosen at RT [29]. The strengthening of enriched nano-
sized oxide particles due to the Orowan mechanism can be
written as Eqs. (1) and (2) [30e32]:
0:81MGb lnð2rs =r0 Þ
sp ¼ (1)
l  2rs
2pð1  nÞ1=2
rffiffiffi " 1=2 #
2 p
l¼2 r 1 (2)
3 4f
where M is the Taylor factor (3.0), G is the shear modulus
(80 GPa), b is the Burgers vector (0.248 nm), l is the mean
planar center to the center distance between nano-sized oxide
particles, n is the Poisson ratio (0.334) [33], r0 is the inner cut-off
radius of a dislocation core, which is assumed to be the
magnitude of the Burgers vector, rs ¼ 0.816
r, r is the mean
planar oxide particles radius of the cross-section of a particle
of radius (3.4 nm and 2.4 nm in 9Cr-non-Zr-ODS steel and 9Cr-
Zr-ODS steel, respectively), and f is the volume fraction of
nano-sized oxide particles (1.02% and 0.62% in 9Cr-non-Zr-
ODS steel and 9Cr-Zr-ODS steel, respectively).
It is well known that grain boundary strengthening is very
important in ultrafine-grained (UFG) materials. In particular,
the present alloy has very fine grain size. Recently, Schneibel
et al. [34] studied the yield stress of ODS alloys with different
microstructures and found that a UFG alloy exhibited much
higher strength than the coarse-grained alloy even at high
temperature. These findings indicated that there is a strong
grain boundary strengthening in ODS steel. Such a grain
boundary strengthening can be best expressed by the
HallePetch relationship as in Eq. (3):
sk ¼ khp d1=2 (3)
pffiffiffi
where khp ¼ 0:2G b[35], and d is average grain size (1.2 mm and
0.8 mm in 9Cr-non-Zr-ODS steel and 9Cr-Zr-ODS steel,
respectively).
In addition to the two aforementioned contributions, solid
a12 ( ) solution strengthening is another contribution in ODS alloys.
Solid solution sss is classically used for ODS alloy with the
90 following form [35, 36]:
X
54 sss ¼ ki XZi (4)
i
184 N u c l e a r E n g i n e e r i n g a n d T e c h n o l o g y 4 9 ( 2 0 1 7 ) 1 7 8 e1 8 8

Fig. 8 e YCrO3 oxide particle. (A) High resolution transmission electron micrograph of YCrO3 oxide particle and its fast
Fourier transformation image in the 9Cr-non-Zr-ODS steel. (B) Fast Fourier transformation filtered image derived from the
image in (A). ODS, oxide dispersion strengthened.

where Xi is the atomic fraction and ki a hardening constant of experiment. The comparison of the results shows that the
the element i, Z ¼ 3/4 for substitutional solid solution (Cr, W), Orowan strengthening mechanism has the largest contribu-
kCr ¼ 9.95 MPa/at%3/4 and kW ¼ 75.79 MPa/at%3/4, respectively. tion among the proposed mechanisms in the ODS steels.
Z ¼ 1/2 for interstitial element (C) is more suitable in body-
centered cubic alloys, kC ¼ 1,122.5 MPa/at%3/4.
4. Discussion
Fig. 14 presents a comparison between the experiment
data and calculation results of RT yield strength. The calcu-
Compared to the 9Cr-Ti-ODS steels with similar composition
lation results are very close to the data measured in the
[22, 37], 9Cr-Zr-ODS steel exhibits finer microstructure and

Fig. 9 e Y4Zr3O12 oxide particles. (A) High resolution transmission electron micrograph of Y4Zr3O12 oxide particles. (B) Fast
Fourier transformation diagram of the micrograph in (A). (C) Fast Fourier transformation filtered image derived from the
image in (A). (D) Simulated SAD pattern from [-210] Y4Zr3O12.. ODS, oxide dispersion strengthened; SAD, selected area
diffraction.
 N u c l e a r E n g i n e e r i n g a n d T e c h n o l o g y 4 9 ( 2 0 1 7 ) 1 7 8 e1 8 8 185

Fig. 10 e YCrO3 oxide particle. (A) High resolution transmission electron micrograph of YCrO3 oxide particle and its fast
Fourier transformation image in the 9Cr-Zr-ODS steel. (B) Fast Fourier transformation filtered image derived from the image
in (A).

Fig. 11 e Tensile stressestrain curves of 9Cr-ODS steels at 25 C and 700 C. (A) 9Cr-non-Zr-ODS steel. (B) 9Cr-Zr-ODS steel.
ODS, oxide dispersion strengthened.

more excellent mechanical properties. The grain size of the 9Cr-
Zr-ODS steel (0.8 mm) is much smaller than 9Cr-Ti-ODS steel
(1.9 mm). The average size and number density of nano-particles
are very close to the 9Cr-Ti-ODS steel. Figs. 15A and 15B show
that the UTS and yield strength of 9Cr-Zr-ODS steel are higher
than 9Cr-Ti-ODS steel at RT and 700 C. According to the first
principle calculation results, compared to the bond lengths
between Y and Ti, the bond lengths is shorten for the defect
clusters containing Zr atoms due to the strong interaction be-
tween Y and Zr. These results suggest that replacing Ti with Zr
leads to higher stability for the nano-oxides [18]. Furthermore,
the Fe-based ODS steels with Zr addition are resistant to grain
growth [14]. In 9Cr-Zr-ODS steel there is UFG and a high number
density of nano-oxides. Some researchers found that UFG-ODS
alloys exhibits unusually high creep resistance at high tem-
perature [38]. The reasons for the good creep resistance in UFG
are attributed to the following factors [39, 40]. Firstly, the self-
diffusion of iron is inhibited due to the fact that the
concentration of individual vacancies is very low in ODS alloys.
Secondly, at the oxide and matrix interfaces, the speed of
interfacial diffusion is very slow due to the fact that the nano-
oxides act as pins that slow the grain boundary diffusion
down. Another important factor is the segregation of W and Cr
at the grain boundaries in ODS alloys. The radius of W atoms is
larger than Fe atoms, which could contribute to slower grain
boundary diffusion.
The capability of ODS steels for long-term nuclear applica-
tions also depends on the irradiation tolerance of the oxides.
Y4Zr3O12 oxide is closely related to cubic fluorite (CaF2) struc-
ture. It is anticipated that Y4Zr3O12 oxide in the Zr-ODS steel is
one of the most radiation-tolerant fluorite structure com-
pounds because it has excellent amorphization resistance and
lower propensities for cluster formation energies than Y2Ti2O7
[41]. This could be one of the most prominent advantages of the
Zr-ODS steel for application in generation IV nuclear fission
reactors and further fusion reactors.
186 N u c l e a r E n g i n e e r i n g a n d T e c h n o l o g y 4 9 ( 2 0 1 7 ) 1 7 8 e1 8 8

Fig. 12 e Tensile properties of 9Cr-ODS steels at 25 C and 700 C. (A) UTS. (B) Total elongation. ODS, oxide dispersion
strengthened; UTS, ultimate tensile strength.

Fig. 13 e SEM rupture micrographs of tensile test specimens at RT. (A) 9Cr-non-Zr ODS steel. (B) 9Cr-Zr-ODS steel. ODS, oxide
dispersion strengthened; RT, room temperature; SEM, scanning electron microscope.

5. Conclusion

The microstructure and mechanical properties of the 9Cr-

Fig. 14 e Comparison of calculated yield strength to
experimental result of oxide dispersion strengthened
steels at room temperature. ODS, oxide dispersion
strengthened.
non-Zr-ODS and 9Cr-Zr-ODS steels were investigated and the
main conclusions are as follows: (1) The grain size of the
9Cr-ODS steel is refined by Zr addition. The grain boundary
maps clearly reveals the existence of subgrain boundaries. (2)
The average size and number density of oxide particles in the
9Cr-Zr-ODS steel are considerably smaller and much higher
than that in the 9Cr-non-Zr-ODS steel. (3) In the 9Cr-Zr-ODS
steel, almost all the particles are Y4Zr3O12 oxide particles, and
the formation of Y2O3 particles is intensively suppressed. (4)
The addition of Zr obviously enhances the mechanical
properties of the 9Cr-ODS steel owing to the formation of
finer Y4Zr3O12 particles, as well as refinement of the matrix
grain. (5) The Orowan mechanism caused by nano-sized
oxide particles is the most important strength mechanism in
the ODS steels.
 N u c l e a r E n g i n e e r i n g a n d T e c h n o l o g y 4 9 ( 2 0 1 7 ) 1 7 8 e1 8 8
Fig. 15 e Strengths of 9Cr-ODS steels at 25 C and 700 C. (A) Ultimate tensile strength of 9Cr-ODS steels. (B) Yield strength of
9Cr-ODS steels. ODS, oxide dispersion strengthened; UTS, ultimate tensile strength; YS, yield strength.
Conflicts of interest
All authors have no conflicts of interest to declare.
Acknowledgments
This research is supported by the National Natural Science
Foundation of China (5147 1049), Fundamental Research
Funds for the Central Universities (N141006001), and Special-
ized Research Fund for the Doctoral Program of Higher Edu-
cation (20130042110014). Haijian Xu is grateful for the financial
support provided by the China Scholarship Council during the
visit to the Hokkaido University, Sapporo 060-8628, Japan.
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