Effect of quasi-hydrostatic extrusion on microhardness in CuCrZr alloy
Effect of quasi-hydrostatic extrusion at liquid nitrogen (77 K) and room (300 K) temperatures on the microhardness in high-strength CuCrZr alloy has been investigated. It is shown that the combination of equalchannel angular compression (ECAP) and quasi-hydrostatic extrusion (QHE) allows raising mic...
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Національний науковий центр «Харківський фізико-технічний інститут» НАН України
2015
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| Cite this: | Effect of quasi-hydrostatic extrusion on microhardness in CuCrZr alloy / A.I. Belyaeva, A.A. Galuza, P.A. Khaimovich, I.V. Kolenov, A.A. Savchenko, I.V. Ryzhkov, A.F. Shtan’, S.I. Solodovchenko, N.A. Shulgin // Вопросы атомной науки и техники. — 2015. — № 1. — С. 170-173. — Бібліогр.: 7 назв. — англ. |
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| author | Belyaeva, A.I. Galuza, A.A. Khaimovich, P.A. Kolenov, I.V. Savchenko, A.A. Ryzhkov, I.V. Shtan’, A.F. Solodovchenko, S.I. Shulgin, N.A. |
| author_facet | Belyaeva, A.I. Galuza, A.A. Khaimovich, P.A. Kolenov, I.V. Savchenko, A.A. Ryzhkov, I.V. Shtan’, A.F. Solodovchenko, S.I. Shulgin, N.A. |
| citation_txt | Effect of quasi-hydrostatic extrusion on microhardness in CuCrZr alloy / A.I. Belyaeva, A.A. Galuza, P.A. Khaimovich, I.V. Kolenov, A.A. Savchenko, I.V. Ryzhkov, A.F. Shtan’, S.I. Solodovchenko, N.A. Shulgin // Вопросы атомной науки и техники. — 2015. — № 1. — С. 170-173. — Бібліогр.: 7 назв. — англ. |
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| container_title | Вопросы атомной науки и техники |
| description | Effect of quasi-hydrostatic extrusion at liquid nitrogen (77 K) and room (300 K) temperatures on the microhardness in high-strength CuCrZr alloy has been investigated. It is shown that the combination of equalchannel angular compression (ECAP) and quasi-hydrostatic extrusion (QHE) allows raising microhardness of CuCrZr alloy especially in the case of the low-temperature (77 K) QHE treatment.
PACS: 68.35.Ct, 81.05.Bx, 81.40.Cd
Исследовано влияние квазигидроэкструзии при температуре жидкого азота (77 K) и комнатной температуре (300 K) на микротвердость жаропрочного CuCrZr-сплава. Выявлено, что комбинация равноканального углового прессования (РКУП) и квазигидроэкструзии (КГЭ) приводит к увеличению микротвердости CuCrZr-сплава, особенно в случае низкотемпературной (77 K) КГЭ-обработки.
Досліджено вплив квазігідроекструзії при температурі рідкого азоту (77 K) та кімнатній температурі (300 K) на мікротвердість жароміцного CuCrZr-сплаву. Визначено, що комбінація рівноканального кутового пресування (РККП) та квазігідроекструзії (КГЕ) призводить до підвищення мікротвердості CuCrZr-сплаву, особливо у випадку низькотемпературної (77 K) КГЕ-обробки.
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| first_indexed | 2025-12-07T18:33:42Z |
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ISSN 1562-6016. ВАНТ. 2015. №1(95)
170 PROBLEMS OF ATOMIC SCIENCE AND TECHNOLOGY. 2015, № 1. Series: Plasma Physics (21), p. 170-173.
EFFECT OF QUASI-HYDROSTATIC EXTRUSION ON
MICROHARDNESS IN CuCrZr ALLOY
A.I. Belyaeva
1
, A.A. Galuza
2
, P.A. Khaimovich
3
, I.V. Kolenov
2
, A.A. Savchenko
1
,
I.V. Ryzhkov
3
, A.F. Shtan’
3
, S.I. Solodovchenko
3
, N.A. Shulgin
3
1
National Technical University “Kharkiv Politechnical Institute”, Kharkiv, Ukraine;
2
Institute of Electrophysics and Radiation Technologies, Kharkiv, Ukraine;
3
NSC‘‘Kharkov Institute of Physics and Technology’’, Kharkov, Ukraine
E-mail: aibelyaeva@mail.ru, alexey.galuza@gmail.com
Effect of quasi-hydrostatic extrusion at liquid nitrogen (77 K) and room (300 K) temperatures on the
microhardness in high-strength CuCrZr alloy has been investigated. It is shown that the combination of equalchannel
angular compression (ECAP) and quasi-hydrostatic extrusion (QHE) allows raising microhardness of CuCrZr alloy
especially in the case of the low-temperature (77 K) QHE treatment.
PACS: 68.35.Ct, 81.05.Bx, 81.40.Cd
INTRODUCTION
Copper and copper alloys are widely used because of
their excellent thermal conductivity, outstanding
resistance to corrosion, ease of fabrication as well as
good strength and fatigue resistance. The high-strength
copper materials take the special place in the
contemporary physical experiments [1]. They are
perspective for the resistance spot welding.
Optimization of the technology of such kind of alloys is
in progress today. Hot hardness is the key property for
such application. In this case the main scientific problem
consists in the necessity to have maximum percent of Cr
precipitations in the copper melt while retaining its high
electro and thermal conductivities with the stabilization
of all physical characteristics.
During the past ten years the ternary Cu-Cr-Zr
system has been widely investigated because of
excellent combination of mechanical strength and
electrical (thermal) conductivity.
Our previous paper [2, 3] has been devoted to
complex investigations of the effect of the structure and
size of grains on changes in the microrelief and optical
characteristics of CuCrZr alloys with substantially
different grain size.
The aim of the present communication is mainly to
study the microstructure and precipitates distribution of
the high-strength Cu-Cr-Zr alloy, in order to get a better
understanding of the strength mechanism and the
composition of the precipitates.
1. MATERIALS AND EXPERIMENTAL
PROCEDURE
The starting material investigated in the present
study was a recently developed precipitation-
strengthened by ECAP light ternary high-strength
commercial Cu-Cr-Zr alloy [2, 3].
Later the starting material was treated by quasi-
hydrostatic extrusion (QHE) at room and cryogenic
temperatures [4].
In the initial state, the starting material was a bar
with a diameter of 20 mm. Cylindrical preforms
~ 4.3 mm in diameter and a length of about 20 mm have
been cut into the longitudinal sections relative to the
axis of the starting bar for subsequent QHE treatment.
Later in the text this direction will be labeled as Lg – the
longitudinal section.
Later these cylindrical preforms were subjected to
QHE at 300 and 77 K. In the text such kind of
treatments are labeled as "QHE300" and "QHE77",
correspondingly. Then the extrudates were cut into
specimens of ~1 2.5 16 mm along the extrudates axis.
Specimens were prepared using standard mechanical
and electrochemical polishing methods to get a high
optical mirror quality. In summary there were the two
specimens for investigation: N1 − (LgQHE300),
N2 − (LgQHE77).
To remove the possible contaminants and the surface
oxides layers after mechanical treatment, the specimens
were cleaned using ions of deuterium plasma (Еi ≈
60 eV/ion; fluence ~2.5 × 10
23
ion/m
2
). The specimens
were sputtered with ions of deuterium plasma having a
wide energy distribution (‹U› = -600 V; j = 2.8 mA/cm
2
;
each exposure, 10 min) [2, 3]. Electron cyclotron
resonance discharge was used for plasma production in
deuterium. In summary one cleaning step and five
sputtering steps were performed.
The microstructures of CuCrZr alloy were examined
by the interferometry and scanning electron microscopy
(SEM). Precipitates in CuCrZr alloy were analyzed by a
JSM-6390LV(JEOL Ltd., Japan) scanning electron
microscope (SEM), equipped with energy dispersive X-
ray spectroscopy (EDXS). Micro-interferometric setup
based on an MII-4 microinterferometer [5] and
multifunctional optic complex [6] were used to
investigate the specimen surface relief.
The standard microhardness tester with load 1H was
used for microhardness analyzing.
2. EXPERIMENTAL RESULTS
The dominating feature of the microstructure of the
CuCrZr alloy after the first sputtering step was the
presence of a relatively high density of Cr-rich
precipitates. After each subsequent sputtering step the
number of precipitates grew. The saturation has been
reached up to fifth sputtering. It means that the sputtered
film eroded by mechanical treatment was taken off.
mailto:aibelyaeva@mail.ru
ISSN 1562-6016. ВАНТ. 2015. №1(95) 171
Fig. 1 reproduces the general feature of the precipitate
microstructure for the two samples after the fifth
sputtering: dots and elongated precipitates (fibers).
a b
Fig. 1. SEM micrograph showing precipitates microstructure of the CuCrZr alloy after the fifth sputtering: (а)
LgQHE300 (N1) and (b) LgQHE77 (N2)
Quasi-hydrostatic extrusion at 77 K leads to more
high dispersive and homogeneous distribution compared
with similar treatment at 300 K (Figs. 1,a,b). That
ensures high precipitate density. As a result, there are
more precipitates in LgQHE77 samples and they are
smaller. This is connected with that the nucleation
centers can not grow through the uniform compression
forces, but there are many precipitates of such kind.
Fig. 2 shows the precipitates distribution and results
of EDXS analysis for a few areas of samples (see
Fig. 2,a). After the fifth sputtering the precipitates with
Cr and Zr enrichments are detected. Analysis of the
matrix shows that it is CuCrZr alloy. The alloy
composition over the sample area is very heterogeneous
(spectrums - insertion to Fig. 2,a). Near Cr clusters the
Cu content reduction takes place in matrix (see Fig. 2,a
spectrum 5) in comparison with distant area.
It should be noted to the special features, connected
with the formation of Zr precipitates. Their number is
much smaller than Cr. The large scale micrograph
(Fig. 2,b) shows fragment of the LgQHE77 sample
surface. The Zr precipitates are marked by the white
arrows. First it is important to note that they look like
parallelepiped in the “crack” of the cooper matrix,
which is attributed to significant distortions of the
crystal lattice. A careful observation of the image (see
Fig. 2,b) revealed some kinds of contrasts associated to
Zr precipitates. One can see the black boundaries of the
crack on the top and from the bottom of the white
parallelepiped - Zr precipitate (see Fig. 2,b). Evidently,
Zr localization in the copper matrix induces large local
lattice distortions of matrix. Specific reason of the crack
formation associated with Zr precipitates remains
unknown to us at present.
Fig. 2,b shows the large scale fragment marked by
the white frame in Fig. 1,b. Zr-rich precipitates which
look like the fibers are indicated by the white arrows.
One can see this image as a line of fibers (or one but
long). For longitudinal samples (both for LgQHE300,
and for LgQHE77) there are large Zr precipitates which
look like elongated precipitates (fibers) having the
lengths ranging from 5 to 50 μm (data not shown here).
It should be noted that the elongated precipitates (fibers)
were formed under ECAP treatment.
Fig. 2. A typical SEM of a large scale micrograph of the
LgQHE77 surface fragment (a); Zr precipitates for
sample LgQHE77 after the fifth sputtering (a large
scale micrograph of the surface fragment marked by the
white frame in Fig. 1,b) (b). Insertions: EDXS analyzes
of the second phases in the areas marked by “+” (wt%)
There are the three phases in the alloy: copper
matrix, Cr-rich phase and Zr-rich phase. A typical
EDXS qualitative analysis spectrum of the Cr-rich phase
is shown in Fig. 3, a (spectrum 5 in the insertion to
Fig. 2,a). There are Cu and Zr peaks besides the Cr
peaks in the spectrum. The EDXS qualitative analysis
172 ISSN 1562-6016. ВАНТ. 2015. №1(95)
results in spectrum 5 (the insertion to Fig. 2,a) shows
that the Cr content of the particle was up to 90.64 wt.%,
so we can suppose that the Cr-rich phase is pure
chromium. Most of the Cr-rich phase is distributed as
little globular particles in a copper matrix. But a few is
distributed as coarse particles (see Fig. 2,a, spectrum 5).
A typical EDXS qualitative analysis spectrum of Zr-
rich phase is shown in Fig. 3 (see Fig. 2,a, spectrum 3).
There are copper, chromium and zirconium peaks. The
zirconium content of the particle was up to 59.85 wt.%.
Almost all of the zirconium-rich phase is distributed as
coarse particles, as precipitates in Fig. 2,a. One should
note that in the present study, Zr precipitates were not
found homogeneously distributed in the matrix.
Fig. 3. A typical EDXS qualitative analysis spectrum in
the areas marked by “+” in Fig. 2,a of: (a) chromium-
rich phase (spectrum 5) and (b) zirconium-rich phase
(spectrum 3). Insertions: EDXS analyzes of the second
phase in the areas marked by “+” in Fig. 2,a
Microhardness of the copper alloy before ECAP, after
ECAP, after QHE300 and QHE77 treatments
Treatment stage Hv, MPa
Before ECAP 1600±30
After ECAP 1820±40
After QHE300 2100±30
After QHE77 2310±30
The microhardness data for the two samples are
displayed in the Table. Provided data are the average of
at least 20 measurements. The Vickers microhardness
(Hv) values ranging from 1600 up to 2310 MPa are
rather large. The data in the Table reflect the
effectiveness of QHE treatment. It is remarkable that
QHE77 treatment ensure higher microhardness in
comparison with the same treatment at 300 K. We have
found that the precipitate density for QHE300 samples
is significantly lower in comparison with QHE77
samples.
3. DISCUSSIONS
The analysis of the experimental data shows that the
nature of the CuCrZr alloy microstructure is connected
with the Cr and Zr precipitates distribution and their
sizes. As described above, there are three phases in the
alloy, Cu matrix, Cr-rich and Zr-rich phases.
The dominating feature of microstructure as revealed
by the SEM investigation is the presence of a relatively
high density of chromium-rich precipitates. It is
concluded that the coarse precipitates mainly consist of
pure chromium. The SEM results indicate that the
precipitate is likely to be pure chromium, with sizes
ranging from 150…700 nm. The average chromuim
precipitate size in the CuCrZr alloy was found to be
460 nm. The content of zirconium in the alloy is reduced
to 0.1 wt.% or less. The possibility visualizing the
microstructure of the alloy under the sputtering process
is based on the fact that the sputtering yields for
precipitates are lower than for the cooper matrix [7]. In
the delivery state the heterogeneous mechanism of
precipitation takes place.
In the present paper at the first time the influence of
the successive employment QHE at liquid nitrogen
(77 K) and room (300 K) temperatures to precipitates
distribution in the prior precipitation-strengthened by
ECAP CuCrZr alloy was investigated. The physical
mechanisms of precipitates distribution in the
precipitation-strengthened CuCrZr alloy after ECAP and
QHE are determined. It is shown that the combination of
ECAP and QHE leads to subsequent grain refinement, to
the alloy structure homogenization and the reduction of
its precipitates size. QHE77 treatment after ECAP leads
to the maximum grain refinement and more
homogeneous distribution of the precipitation compared
with QHE300, which is connected with retardation of
the diffusion process and recrystallisation for the second
time at low temperature.
As it is shown above in the Table the QHE77
treatment ensures higher microhardness (~2300 MPa) in
comparison with the same treatment at 300 K. This fact
reflects the precipitates density in the samples. It is
higher for QHE77 in comparison with the QHE300
treatment. This result is correlated with microstructure
data which is connected with the homogeneous
distribution of Cr precipitates.
The spatial distribution of the precipitates was found
to be fairly homogeneous throughout the whole volume
and there were no significant variations in the size and
density of precipitates over the surface. The precipitate
density increasing is connected with the stress growth.
The crack formation is a result of this process. Along
these cracks through the high stress the precipitates dots
transform into the elongation strips with high density.
The density of inclusions became so high that many
combined with adjacent ones, forming a system of
oblong curved hillock-type defects. It is lead to local
inhomogeneity on the sample surface.
As a consequence, one may conclude the following.
If the cooper matrix grains are much larger than the size
of the second phase particles, precipitates Cr and Zr are
localized prior over the grain boundaries. It is shown
ISSN 1562-6016. ВАНТ. 2015. №1(95) 173
that the grain boundaries are the most effective
concentrators for precipitators at the grain size
~30…40 μm [2, 3]. The result of the present paper
shows, that the grain size of cooper matrix is much less
than the precipitate size. In this case the nucleation
center of the Cr and Zr precipitates are determined by
the defects and dislocations in the samples. As a result
of QHE grain size is <100 nm and the homogeneous
distribution of precipitates takes place: precipitate
distribution is determined only by the dislocations and
other defects. The later distribution determines the
topography and the surface roughness. It is noteworthy
that the combination of equal-channel angular
compression (ECAP) and quasi-hydrostatic extrusion
(QHE) allows raising microhardness of CuCrZr alloy
especially in the case of the QHE77 treatment.
CONCLUSIONS
Effect of quasi-hydrostatic extrusion at liquid
nitrogen (77 K) and room (300 K) temperatures on the
structure formation of preliminary dispersion-
strengthened CuCrZr alloy has been investigated in this
communication. The sputtering process with deuterium
ions was chosen as an instrument for examining the
alloy structure. The main peculiarity of microstructure is
connected with the high density of small chromium
precipitates. It is shown that the combination of equal-
channel angular compression (ECAP) and quasi-
hydrostatic extrusion (QHE) allows raising micro
hardness of CuCrZr alloy especially under low-
temperature QHE77 treatment up to 2300 MPa.
REFERENCES
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investigation of Cr precipitation in copper // Acta
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A.A. Galuza, D.A. Aksenov, S.N. Faizova,
V.S. Voitsenya, V.G. Konovalov, I.V. Ryzhkov,
O.A. Skorik, S.I. Solodovchenko, A.F. Bardamid.
Influence of grain size on stability under ion sputtering
of Cu-Cr-Zr copper alloy mirrors // Problems of Atomic
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2011, №4, p. 50-59.
3. A.I. Belyaeva, A.A. Galuza, I.V. Kolenov,
A.A. Savchenko, S.N. Faizova, G.N. Raab,
D.A. Aksenov. Effect of Microrelief on the Optical
Characteristics of Light Cr-Zr Copper Alloys
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5. A.I. Belyaeva, A.A. Galuza, A.D. Kudlenko.
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6. A.I. Belyaeva, A.A. Galuza, I.V. Kolenov,
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and alloys surface // Problems of Atomic Science and
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Article received 02.12.2014
ВЛИЯНИЕ КВАЗИГИДРОЭКСТРУЗИИ НА МИКРОТВЕРДОСТЬ СПЛАВА CuCrZr
А.И. Беляева, A.A. Галуза, П.А. Хаймович, И.В. Коленов, A.A. Савченко, И.В. Рыжков, А.Ф. Штань,
С.И. Солодовченко, Н.A. Шульгин
Исследовано влияние квазигидроэкструзии при температуре жидкого азота (77 K) и комнатной
температуре (300 K) на микротвердость жаропрочного CuCrZr-сплава. Выявлено, что комбинация
равноканального углового прессования (РКУП) и квазигидроэкструзии (КГЭ) приводит к увеличению
микротвердости CuCrZr-сплава, особенно в случае низкотемпературной (77 K) КГЭ-обработки.
ВПЛИВ КВАЗІГІДРОЕКСТРУЗІЇ НА МІКРОТВЕРДІСТЬ СПЛАВУ CuCrZr
А.І. Беляєва, A.A. Галуза, П.А. Хаймовіч, И.В. Коленов, A.A. Савченко, І.В. Рижков, А.Ф. Штань,
С.І. Солодовченко, Н.A. Шульгин
Досліджено вплив квазігідроекструзії при температурі рідкого азоту (77 K) та кімнатній температурі
(300 K) на мікротвердість жароміцного CuCrZr-сплаву. Визначено, що комбінація рівноканального кутового
пресування (РККП) та квазігідроекструзії (КГЕ) призводить до підвищення мікротвердості CuCrZr-сплаву,
особливо у випадку низькотемпературної (77 K) КГЕ-обробки.
|
| id | nasplib_isofts_kiev_ua-123456789-82143 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1562-6016 |
| language | English |
| last_indexed | 2025-12-07T18:33:42Z |
| publishDate | 2015 |
| publisher | Національний науковий центр «Харківський фізико-технічний інститут» НАН України |
| record_format | dspace |
| spelling | Belyaeva, A.I. Galuza, A.A. Khaimovich, P.A. Kolenov, I.V. Savchenko, A.A. Ryzhkov, I.V. Shtan’, A.F. Solodovchenko, S.I. Shulgin, N.A. 2015-05-25T15:27:02Z 2015-05-25T15:27:02Z 2015 Effect of quasi-hydrostatic extrusion on microhardness in CuCrZr alloy / A.I. Belyaeva, A.A. Galuza, P.A. Khaimovich, I.V. Kolenov, A.A. Savchenko, I.V. Ryzhkov, A.F. Shtan’, S.I. Solodovchenko, N.A. Shulgin // Вопросы атомной науки и техники. — 2015. — № 1. — С. 170-173. — Бібліогр.: 7 назв. — англ. 1562-6016 PACS: 68.35.Ct, 81.05.Bx, 81.40.Cd https://nasplib.isofts.kiev.ua/handle/123456789/82143 Effect of quasi-hydrostatic extrusion at liquid nitrogen (77 K) and room (300 K) temperatures on the microhardness in high-strength CuCrZr alloy has been investigated. It is shown that the combination of equalchannel angular compression (ECAP) and quasi-hydrostatic extrusion (QHE) allows raising microhardness of CuCrZr alloy especially in the case of the low-temperature (77 K) QHE treatment.
 PACS: 68.35.Ct, 81.05.Bx, 81.40.Cd Исследовано влияние квазигидроэкструзии при температуре жидкого азота (77 K) и комнатной температуре (300 K) на микротвердость жаропрочного CuCrZr-сплава. Выявлено, что комбинация равноканального углового прессования (РКУП) и квазигидроэкструзии (КГЭ) приводит к увеличению микротвердости CuCrZr-сплава, особенно в случае низкотемпературной (77 K) КГЭ-обработки. Досліджено вплив квазігідроекструзії при температурі рідкого азоту (77 K) та кімнатній температурі (300 K) на мікротвердість жароміцного CuCrZr-сплаву. Визначено, що комбінація рівноканального кутового пресування (РККП) та квазігідроекструзії (КГЕ) призводить до підвищення мікротвердості CuCrZr-сплаву, особливо у випадку низькотемпературної (77 K) КГЕ-обробки. en Національний науковий центр «Харківський фізико-технічний інститут» НАН України Вопросы атомной науки и техники Низкотемпературная плазма и плазменные технологии Effect of quasi-hydrostatic extrusion on microhardness in CuCrZr alloy Влияние квазигидроэкструзии на микротвердость сплава CuCrZr Вплив квазігідроекструзії на мікротвердість сплаву CuCrZr Article published earlier |
| spellingShingle | Effect of quasi-hydrostatic extrusion on microhardness in CuCrZr alloy Belyaeva, A.I. Galuza, A.A. Khaimovich, P.A. Kolenov, I.V. Savchenko, A.A. Ryzhkov, I.V. Shtan’, A.F. Solodovchenko, S.I. Shulgin, N.A. Низкотемпературная плазма и плазменные технологии |
| title | Effect of quasi-hydrostatic extrusion on microhardness in CuCrZr alloy |
| title_alt | Влияние квазигидроэкструзии на микротвердость сплава CuCrZr Вплив квазігідроекструзії на мікротвердість сплаву CuCrZr |
| title_full | Effect of quasi-hydrostatic extrusion on microhardness in CuCrZr alloy |
| title_fullStr | Effect of quasi-hydrostatic extrusion on microhardness in CuCrZr alloy |
| title_full_unstemmed | Effect of quasi-hydrostatic extrusion on microhardness in CuCrZr alloy |
| title_short | Effect of quasi-hydrostatic extrusion on microhardness in CuCrZr alloy |
| title_sort | effect of quasi-hydrostatic extrusion on microhardness in cucrzr alloy |
| topic | Низкотемпературная плазма и плазменные технологии |
| topic_facet | Низкотемпературная плазма и плазменные технологии |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/82143 |
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