Effect of hydrogenation on creep and structure evolution of nanocrystalline Zr1Nb alloy
The regularities of creep, mechanical characteristics, and structure evolution of Zr1Nb nanocrystalline alloy obtained by intensive plastic deformation and hydrogenated from a gaseous medium are studied. It is shown that, due to deformation under creep conditions, a small amount of zirconium hydride...
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| Опубліковано в: : | Problems of Atomic Science and Technology |
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Національний науковий центр «Харківський фізико-технічний інститут» НАН України
2023
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| Цитувати: | Effect of hydrogenation on creep and structure evolution of nanocrystalline Zr1Nb alloy / E.S. Savchuk, V.I. Sokolenko, E.V. Karaseva, A.V. Mats, V.A. Frolov, M.M. Pylypenko // Problems of Atomic Science and Technology. — 2023. — № 2. — С. 64-68. — Бібліогр.: 14 назв. — англ. |
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Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1860239750571491328 |
|---|---|
| author | Savchuk, E.S. Sokolenko, V.I. Karaseva, E.V. Mats, A.V. Frolov, V.A. Pylypenko, M.M. |
| author_facet | Savchuk, E.S. Sokolenko, V.I. Karaseva, E.V. Mats, A.V. Frolov, V.A. Pylypenko, M.M. |
| citation_txt | Effect of hydrogenation on creep and structure evolution of nanocrystalline Zr1Nb alloy / E.S. Savchuk, V.I. Sokolenko, E.V. Karaseva, A.V. Mats, V.A. Frolov, M.M. Pylypenko // Problems of Atomic Science and Technology. — 2023. — № 2. — С. 64-68. — Бібліогр.: 14 назв. — англ. |
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| container_title | Problems of Atomic Science and Technology |
| description | The regularities of creep, mechanical characteristics, and structure evolution of Zr1Nb nanocrystalline alloy obtained by intensive plastic deformation and hydrogenated from a gaseous medium are studied. It is shown that, due to deformation under creep conditions, a small amount of zirconium hydrides is formed in the structure of the Zr1Nb alloy, which has little effect on its strength properties and ductility. The observed features of the creep characteristics are mainly due to the past relaxation of internal stresses and the corresponding structural transformations during hydrogenation and subsequent deformation.
Досліджено закономірності повзучості, механічні характеристики та еволюцію структури нанокристалічного сплаву Zr1Nb, отриманого шляхом інтенсивної пластичної деформації та насиченого воднем з газового середовища. Показано, що внаслідок деформації в умовах повзучості в структурі сплаву Zr1Nb утворюється невелика кількість гідридів цирконію, що мало впливає на його міцнісні властивості та пластичність. Спостережувані особливості характеристик повзучості зумовлені в основному релаксацією внутрішніх напружень і відповідними структурними перетвореннями під час наводнювання та подальшої деформації.
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64 ISSN 1562-6016. Problems of Atomic Science and Technology. 2023. №2(144)
https://doi.org/10.46813/2023-144-064
EFFECT OF HYDROGENATION ON CREEP AND STRUCTURE
EVOLUTION OF NANOCRYSTALLINE Zr1Nb ALLOY
E.S. Savchuk, V.I. Sokolenko, E.V. Karaseva, A.V. Mats, V.A. Frolov, M.M. Pylypenko
National Science Center “Kharkov Institute of Physics and Technology”,
Kharkiv, Ukraine
Е-mail: vsokol@kipt.kharkov.ua
The regularities of creep, mechanical characteristics, and structure evolution of Zr1Nb nanocrystalline alloy
obtained by intensive plastic deformation and hydrogenated from a gaseous medium are studied. It is shown that,
due to deformation under creep conditions, a small amount of zirconium hydrides is formed in the structure of the
Zr1Nb alloy, which has little effect on its strength properties and ductility. The observed features of the creep
characteristics are mainly due to the past relaxation of internal stresses and the corresponding structural
transformations during hydrogenation and subsequent deformation.
PACS: 62.20.Hg, 61.72.Ff, 61.10.-i
INTRODUCTION
Zirconium alloys are widely used in the nuclear
power industry as а structural materials for fuel rod
cladding in nuclear reactors. During exploitation, the
fuel rod claddings operate in difficult conditions with
the simultaneous action of irradiation, high temperature,
corrosive environment and mechanical stresses [1, 2].
Therefore, the fuel rod cladding material must have
good mechanical properties, corrosion resistance, and
radiation growth resistance.
The critical processes that limit the service life of
reactor materials include their hydrogenation [3].
Hydrogen diffusing in the crystal lattice of a metal is
able to interact with various kinds of defects contained
in real solids [3, 4]. The hydrogenation of metals
strongly depends on the deformation of the lattice, the
nature of the dislocation structure, and the appearance
of point defects. Deformation can lead to a decrease or
increase in the volume of hydrogen collectors, and,
accordingly, change the absorption capacity of metals.
In this case, microcavities and blisters have the greatest
effect on the capture of hydrogen [4, 5].
Hydrogen, either in a solid solution or in the form of
a hydride, causes embrittlement of metals and alloys.
Hydrogen embrittlement of zirconium alloys is one of
the most important safety issues for nuclear power
plants using light water reactors and the main cause of
mechanical degradation of fuel cladding [6–8].
Hydride precipitates reduce the ability of the
material to plastic deformation and reduce its crack
resistance. The degree of reduction in the plasticity of a
hydrogenated alloy depends on the concentration of
hydrogen, temperature, size, morphology of hydrides
and their orientation with respect to the applied stresses.
In this case, the factors of temperature and orientation
are most often decisive. The greatest embrittlement is
caused by lamellar precipitates oriented perpendicular to
the direction of acting stresses [6]. The formation of
hydrides leads to the formation of microcracks at
interfacial boundaries.
Studies have shown that hydrogen does not
significantly affect the strength characteristics of
zirconium and its alloys, but considerably reduces its
impact strength at low temperatures. Hydrogen
embrittlement manifests itself at a content of 0.001% H2
and manifests itself more intensely, the higher the
hydrogen content [7, 8].
The purpose of this work is to study the regularities
of creep and evolution of the nanostructure of the
Zr1Nb alloy obtained by intensive plastic deformation
(IPD) and the effect on its mechanical characteristics
and structure of hydrogenation.
MATERIAL AND PROCESSING METHOD
An ingot of Zr1Nb alloy obtained by electron beam
melting was cut into templates and deformed by
combined rolling at 77…300 K to the true strain value
of ~ 3.9. Samples 3×0.2×50 mm in size were
mechanically cut from rolled strips. The chemical
composition of the alloy under study is given in [9]. In
order to study the effect of hydrogenation on the
structure and properties of the alloy, processing was
carried out in the following modes:
1. MT-1 – rolling deformation, final strain ~ 3.9;
2. MT-2 – MT-1 + hydrogenation.
Samples were saturated with hydrogen on an
automated setup based on a helium leak detector. The
sample was placed in a chamber, the pressure in which
was pumped out to 0.013 Pa, after which hydrogen was
injected into it at a pressure of ~ 0.05 MPa. The sample
was continuously heated at a rate of 8 K/min to a
temperature of 680 K, kept at this temperature for 5 h,
and the pressure in the chamber was measured. The
amount of absorbed gas was determined from the
pressure difference in the chamber before and after
saturation by the gravimetric method, as well as from
the dependence of the intensity of hydrogen yield on
temperature during uniform heating of the samples, and
its amounted to 0.09 wt.%
Creep tests were carried out in the step loading
regime at a temperature of 300 and 680 K, the
measurement accuracy was ~ 510
-5
cm. The electrical
resistance (R) was measured at room temperature by the
compensation method. The structure evolution control
was carried out using the electron microscopic method.
mailto:vsokol@kipt.kharkov.ua
ISSN 1562-6016. Problems of Atomic Science and Technology. 2023. №2(144) 65
RESULTS AND DISCUSSION
Fig. 1 and Table show the dependences of the
creep rate at 300 and 680 K and the mechanical
characteristics of Zr1Nb alloy samples after rolling
and after hydrogenation in the entire studied stress
range.
Fig. 1. Creep rates at Т = 300 К (3, 4) and 680 К (1, 2)
as a function of the true stress for the samples of Zr1Nb
alloy subjected to different treatments:
1, 3 – МT-1; 2, 4 – МT–2
Mechanical characteristics of Zr1Nb alloy samples after
various treatments
Fig. 2. TEM images of Zr1Nb alloy after following
treatments: a – MT-1; b – MT-1+creep at 680 К
(σ 0.9σВ)
It can be seen from the above figure and table that
hydrogenation to 0.09 wt.% of samples of the deformed
Zr1Nb alloy when tested under creep conditions at
300 K leads to a decrease in the strength characteristics
of the samples, but a plasticity does not change. In the
process of creep at 680 K after hydrogenation, the
strength characteristics and plasticity change slightly
compared to the characteristics of the samples of the
deformed alloy, however, it should be noted that the
strength properties tend to increase.
Structural studies have shown that after combined
rolling of the Zr1Nb alloy by a true strain value of
ε ~ 3.9, a nanostructure with a grain size of ~ 60 nm is
formed. The density of dislocations in the body of
grains is ~ 3.410
10
cm
-2
. The main amount of
dislocations is concentrated at the grain boundaries and
triple junctions. The average size of misorientations
caused by the boundaries is ~ 6
0
. In this case, a high
concentration of high-angle boundaries (8…30
0
), as
well as dangling dislocation boundaries, is observed.
The sharp inhomogeneity of the contrast in the electron
microscope images indicates a high level of internal
stresses and the presence of peak stresses at the junction
of boundaries (Fig. 2,а).
The nanostructure created by IPD rolling turned out
to be unstable to subsequent mechanical and thermal
effects under creep conditions at 680 K (see Fig. 2,b).
Most of the boundaries collapsed and in their place
dislocation boundaries of the polygonal type were
formed. The polygon sizes range from 50…150 nm.
Extended boundaries with large, above 200,
disorientation angles have been partially preserved.
When we studying the mechanisms of plastic flow
of the nanostructured Zr1Nb alloy obtained using IPD,
we showed [10–13] that plastic deformation occurs due
to the transformation of the initial structure by the
activation of recovery processes: dislocation climbing at
the grain boundaries, the processes of generation and
annihilation of dislocations at the boundaries, which
leads to their scattering and is accompanied by stress
relaxation. This process includes the destruction of the
original structural configuration created as a result of
rolling and the formation of a new structure that is less
stressed and more resistant to subsequent deformation.
The reason for the occurrence of the kinetic instability
of the deformation structure is a changes in the
geometry of plastic deformation and in the temperature-
speed regime of deformation.
The reaction of the structure to annealing in a
hydrogen atmosphere is nonuniform over the sample
volume. In most places, recrystallization processes have
taken place. This is the completed primary
recrystallization, as well as collective recrystallization.
However, polygonal boundaries are also visible. In
other volumes, initial recovery processes in the
crystalline and boundary phases with partial destruction
of the deformation structure were revealed.
The size of new grains varies within a wide range of
0.08…0.5 µm, but can reach ~ 2 µm. Such a sharp
inhomogeneity of the recrystallized structure is called
island inhomogeneity and can lead to changes in
mechanical properties (Fig. 3,a,b). According to the
state diagram of Zr-H [14], at a concentration of
0.09 wt.%, the amount of the δ-phase in the α-matrix is
insignificant and, therefore, is not resolute by our
methods.
Test
temperature
Modes of
treatment
R300/R77
σ0.2,
МPа
σB,
МPа
ε, %
300 К
МО-1 3.52 812 890 7.3
МО-1+Н2 3.86 567 685 7.4
680 К
МО-1 3.52 187 273 10.9
МО-1+Н2 3.86 201 305 11.0
66 ISSN 1562-6016. Problems of Atomic Science and Technology. 2023. №2(144)
Fig. 3. TEM images of Zr1Nb alloy after following
treatments: a, b – MT-2; c, d – MT-2+creep at
680 К (σ 0.9σВ)
The structure after creep at 680 K at the end of the
uniform tensile region of the samples (σ 0.9σB) is
inhomogeneous. In the recrystallized microregions, the
processes characteristic of tension at elevated
temperatures took place – the accumulation of
dislocations with the formation of dislocation
boundaries framing cells and fragments. In the volumes
not affected by the processes of polygonization and
recrystallization, intensive dynamic recrystallization
took place (d = 0.05…1 μm) (see Fig. 3,c,d).
Fig. 4. TEM images of the Zr1Nb alloy after MT-2
and creep at 680 K (σ 0.9σВ) having the precipitation
of hydrides. Bright-field image of the structure (a);
microdiffraction from an area of 2 μm
2
(b); dark-field
image in reflection (311) (c); reflex and precipitate are
shown by black and white arrows, respectively
The action of tensile loads during creep initiates the
formation of zirconium hydrides – this is a δ-phase with
an fcc lattice and contains up to 55 at.% hydrogen.
Individual sparsely spaced hydride precipitates, which
do not interact with each other and are separated from
the matrix by boundaries with a low degree of
coherence, are short-range barriers for mobile
dislocations (Fig. 4). The formation of such particles is
possible in places of large structural discrepancy, which
are powerful channel for hydrogen atoms and places of
their excessive concentration.
The plastic flow in the region of macrolocalization is
very inhomogeneous. Plastic deformation through the
formation and displacement of new boundaries is
carried out under conditions of dominant
crystallographic anisotropy – a sharp rolling texture.
ISSN 1562-6016. Problems of Atomic Science and Technology. 2023. №2(144) 67
The recrystallization texture repeats the deformation
texture, where the number of other admitted slip
systems is sharply limited and the translational mode of
dislocations is quickly exhausted.
Upon completion of primary recrystallization, when
a critical concentration of structural discrepancy (triple
junctions of boundaries) is reached, macrolocalization
in the form of a “neck” is initiated. This means that the
rate of plastic relaxation becomes less than the rate of
plastic deformation. Usually, along with the formation
of a dislocation and finely fragmented structure that is
stable up to destruction, processes of dynamic
recrystallization actively proceed, where microcracks
are formed at the so-called critical junctions of grain
boundaries. In our case, nuclei of secondary
recrystallization are formed. Their size is less than
50 nm.
The growth of secondary grains is carried out under
conditions of accelerated plastic flow and a gradual
decrease in the structural elements of deformation.
Finally, the formation of a new dissipative structure
ends with the loss of stability of the entire system with
the formation of delamination cracks at the junctions of
new boundaries and destruction of the sample (Fig. 5).
Fig. 5. TEM images in the area of pre-fracture of the
Zr1Nb alloy after MT-2 during creep at 680 K.
The arrow shows the initiation of discontinuities
An analysis of the obtained results shows that the
observed features of the mechanical characteristics of
the Zr1Nb alloy after the studied impacts are due to the
characteristics of the obtained structures. Thus, a
decrease in strength characteristics during creep tests at
300 K for samples of the Zr1Nb nanostructured alloy
hydrogenated at 680 K for 5 h is a result, of a decrease
in internal stresses. This is evidenced by the observed
structural changes: polygonization, recrystallization,
grain growth. However, the plasticity of the material did
not change, which may be due to the strong
inhomogeneity of the recrystallized structure.
At 680 K, the mechanical characteristics of the
samples after rolling and after hydrogenation were
almost the same. This may be a consequence, on the one
hand, of the strong kinetic instability of the
nanostructure obtained by rolling, as was shown earlier
[10–13]. On the other hand, the structure recrystallized
in the process of hydrogenation is inhomogeneous and,
during creep, hydride precipitates with incoherent
boundaries are formed in it, which are powerful
obstacles in the way of dislocation glide. As a result,
there is a slight increase in the strength properties of
hydrogenated samples.
CONCLUSIONS
The regularities of creep, mechanical characteristics,
and evolution of the structure of the nanocrystalline
Zr1Nb alloy obtained by intensive plastic deformation
and hydrogenated from a gaseous medium are studied.
It is shown that due to hydrogenation up to
0.09 wt.% and subsequent deformation under creep
conditions, a small amount of hydrides is formed, which
have little effect on the strength characteristics and
plasticity of the Zr1Nb alloy.
The observed features of the mechanical
characteristics of the hydrogenated nanostructured
Zr1Nb alloy are mainly due to the past relaxation of
internal stresses and the corresponding structural
transformations during hydrogenation and subsequent
creep.
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Article received 17.03.2023
ВПЛИВ НАВОДНЮВАННЯ НА ПОВЗУЧІСТЬ ТА ЕВОЛЮЦІЮ СТРУКТУРИ
НАНОКРИСТАЛІЧНОГО СПЛАВУ Zr1Nb
Є.С. Савчук, В.І. Соколенко, Є.В. Карасьова, О.В. Мац, В.О. Фролов, М.М. Пилипенко
Досліджено закономірності повзучості, механічні характеристики та еволюцію структури
нанокристалічного сплаву Zr1Nb, отриманого шляхом інтенсивної пластичної деформації та насиченого
воднем з газового середовища. Показано, що внаслідок деформації в умовах повзучості в структурі сплаву
Zr1Nb утворюється невелика кількість гідридів цирконію, що мало впливає на його міцнісні властивості та
пластичність. Спостережувані особливості характеристик повзучості зумовлені в основному релаксацією
внутрішніх напружень і відповідними структурними перетвореннями під час наводнювання та подальшої
деформації.
|
| id | nasplib_isofts_kiev_ua-123456789-196105 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1562-6016 |
| language | English |
| last_indexed | 2025-12-07T18:28:42Z |
| publishDate | 2023 |
| publisher | Національний науковий центр «Харківський фізико-технічний інститут» НАН України |
| record_format | dspace |
| spelling | Savchuk, E.S. Sokolenko, V.I. Karaseva, E.V. Mats, A.V. Frolov, V.A. Pylypenko, M.M. 2023-12-10T12:55:48Z 2023-12-10T12:55:48Z 2023 Effect of hydrogenation on creep and structure evolution of nanocrystalline Zr1Nb alloy / E.S. Savchuk, V.I. Sokolenko, E.V. Karaseva, A.V. Mats, V.A. Frolov, M.M. Pylypenko // Problems of Atomic Science and Technology. — 2023. — № 2. — С. 64-68. — Бібліогр.: 14 назв. — англ. 1562-6016 PACS: 62.20.Hg, 61.72.Ff, 61.10.-i DOI: https://doi.org/10.46813/2023-144-064 https://nasplib.isofts.kiev.ua/handle/123456789/196105 The regularities of creep, mechanical characteristics, and structure evolution of Zr1Nb nanocrystalline alloy obtained by intensive plastic deformation and hydrogenated from a gaseous medium are studied. It is shown that, due to deformation under creep conditions, a small amount of zirconium hydrides is formed in the structure of the Zr1Nb alloy, which has little effect on its strength properties and ductility. The observed features of the creep characteristics are mainly due to the past relaxation of internal stresses and the corresponding structural transformations during hydrogenation and subsequent deformation. Досліджено закономірності повзучості, механічні характеристики та еволюцію структури нанокристалічного сплаву Zr1Nb, отриманого шляхом інтенсивної пластичної деформації та насиченого воднем з газового середовища. Показано, що внаслідок деформації в умовах повзучості в структурі сплаву Zr1Nb утворюється невелика кількість гідридів цирконію, що мало впливає на його міцнісні властивості та пластичність. Спостережувані особливості характеристик повзучості зумовлені в основному релаксацією внутрішніх напружень і відповідними структурними перетвореннями під час наводнювання та подальшої деформації. en Національний науковий центр «Харківський фізико-технічний інститут» НАН України Problems of Atomic Science and Technology Thermal and fast reactor materials Effect of hydrogenation on creep and structure evolution of nanocrystalline Zr1Nb alloy Вплив наводнювання на повзучість та еволюцію структури нанокристалічного сплаву Zr1Nb Article published earlier |
| spellingShingle | Effect of hydrogenation on creep and structure evolution of nanocrystalline Zr1Nb alloy Savchuk, E.S. Sokolenko, V.I. Karaseva, E.V. Mats, A.V. Frolov, V.A. Pylypenko, M.M. Thermal and fast reactor materials |
| title | Effect of hydrogenation on creep and structure evolution of nanocrystalline Zr1Nb alloy |
| title_alt | Вплив наводнювання на повзучість та еволюцію структури нанокристалічного сплаву Zr1Nb |
| title_full | Effect of hydrogenation on creep and structure evolution of nanocrystalline Zr1Nb alloy |
| title_fullStr | Effect of hydrogenation on creep and structure evolution of nanocrystalline Zr1Nb alloy |
| title_full_unstemmed | Effect of hydrogenation on creep and structure evolution of nanocrystalline Zr1Nb alloy |
| title_short | Effect of hydrogenation on creep and structure evolution of nanocrystalline Zr1Nb alloy |
| title_sort | effect of hydrogenation on creep and structure evolution of nanocrystalline zr1nb alloy |
| topic | Thermal and fast reactor materials |
| topic_facet | Thermal and fast reactor materials |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/196105 |
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