Microstructure Investigation of the Spark Plasma Sintered Cu—Al—Ni Shape Memory Material
Исследована микроструктура компактов Cu—13,0Al—3,9Ni—0,4Ti—0,2Cr масс.%, спечённых плазменно-искровым методом из электроэрозионных порошков, изготовленных из мастер-сплава в жидком аргоне. Досліджено мікроструктуру компактів Cu—13,0Al—3,9Ni—0,4Ti—0,2Cr ваг.% спечених плазмово-іскровим методом із еле...
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Інститут металофізики ім. Г.В. Курдюмова НАН України
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| Cite this: | Microstructure Investigation of the Spark Plasma Sintered Cu—Al—Ni Shape Memory Material / G.E. Monastyrsky, A.V. Kotko, A.V. Gilchuk, P. Ochin, V.I Kolomytsev., Yu.N. Koval // Металлофизика и новейшие технологии. — 2014. — Т. 36, № 8. — С. 1091-1099. — Бібліогр.: 18 назв. — англ. |
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Monastyrsky, G.E. Kotko, A.V. Gilchuk, A.V. Ochin, P. Kolomytsev, V.I. Koval, Yu.N. 2016-10-10T19:16:21Z 2016-10-10T19:16:21Z 2014 Microstructure Investigation of the Spark Plasma Sintered Cu—Al—Ni Shape Memory Material / G.E. Monastyrsky, A.V. Kotko, A.V. Gilchuk, P. Ochin, V.I Kolomytsev., Yu.N. Koval // Металлофизика и новейшие технологии. — 2014. — Т. 36, № 8. — С. 1091-1099. — Бібліогр.: 18 назв. — англ. 1024-1809 PACS: 81.05.Bx, 81.07.Bc, 81.07.Wx, 81.20.Ev, 81.30.Kf, 81.30.Mh DOI: http://dx.doi.org/10.15407/mfint.36.08.1091 https://nasplib.isofts.kiev.ua/handle/123456789/106997 Исследована микроструктура компактов Cu—13,0Al—3,9Ni—0,4Ti—0,2Cr масс.%, спечённых плазменно-искровым методом из электроэрозионных порошков, изготовленных из мастер-сплава в жидком аргоне. Досліджено мікроструктуру компактів Cu—13,0Al—3,9Ni—0,4Ti—0,2Cr ваг.% спечених плазмово-іскровим методом із електроерозійних порошків, виготовлених із мастер-стопу в рідкому арґоні. The microstructure of Cu—13.0Al—3.9Ni—0.4Ti—0.2Cr wt.% compacts sintered by spark plasma method from powders prepared by spark-erosion method in liquid argon from master alloy is investigated. Authors appreciate Prof. G. S. Oliynyk for the consultation and assistance in the Ar ions etching of the SPS samples for TEM investigation. en Інститут металофізики ім. Г.В. Курдюмова НАН України Металлофизика и новейшие технологии Дефекты кристаллической решётки Microstructure Investigation of the Spark Plasma Sintered Cu—Al—Ni Shape Memory Material Исследование микроструктуры материала Cu—Al—Ni с памятью формы, спечённого плазменно-искровым методом Дослідження мікроструктури матеріалу Cu—Al—Ni з пам’яттю форми, спеченого плазмово-іскровим методом Article published earlier |
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| title |
Microstructure Investigation of the Spark Plasma Sintered Cu—Al—Ni Shape Memory Material |
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Microstructure Investigation of the Spark Plasma Sintered Cu—Al—Ni Shape Memory Material Monastyrsky, G.E. Kotko, A.V. Gilchuk, A.V. Ochin, P. Kolomytsev, V.I. Koval, Yu.N. Дефекты кристаллической решётки |
| title_short |
Microstructure Investigation of the Spark Plasma Sintered Cu—Al—Ni Shape Memory Material |
| title_full |
Microstructure Investigation of the Spark Plasma Sintered Cu—Al—Ni Shape Memory Material |
| title_fullStr |
Microstructure Investigation of the Spark Plasma Sintered Cu—Al—Ni Shape Memory Material |
| title_full_unstemmed |
Microstructure Investigation of the Spark Plasma Sintered Cu—Al—Ni Shape Memory Material |
| title_sort |
microstructure investigation of the spark plasma sintered cu—al—ni shape memory material |
| author |
Monastyrsky, G.E. Kotko, A.V. Gilchuk, A.V. Ochin, P. Kolomytsev, V.I. Koval, Yu.N. |
| author_facet |
Monastyrsky, G.E. Kotko, A.V. Gilchuk, A.V. Ochin, P. Kolomytsev, V.I. Koval, Yu.N. |
| topic |
Дефекты кристаллической решётки |
| topic_facet |
Дефекты кристаллической решётки |
| publishDate |
2014 |
| language |
English |
| container_title |
Металлофизика и новейшие технологии |
| publisher |
Інститут металофізики ім. Г.В. Курдюмова НАН України |
| format |
Article |
| title_alt |
Исследование микроструктуры материала Cu—Al—Ni с памятью формы, спечённого плазменно-искровым методом Дослідження мікроструктури матеріалу Cu—Al—Ni з пам’яттю форми, спеченого плазмово-іскровим методом |
| description |
Исследована микроструктура компактов Cu—13,0Al—3,9Ni—0,4Ti—0,2Cr масс.%, спечённых плазменно-искровым методом из электроэрозионных порошков, изготовленных из мастер-сплава в жидком аргоне.
Досліджено мікроструктуру компактів Cu—13,0Al—3,9Ni—0,4Ti—0,2Cr ваг.% спечених плазмово-іскровим методом із електроерозійних порошків, виготовлених із мастер-стопу в рідкому арґоні.
The microstructure of Cu—13.0Al—3.9Ni—0.4Ti—0.2Cr wt.% compacts sintered by spark plasma method from powders prepared by spark-erosion method in liquid argon from master alloy is investigated.
|
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1024-1809 |
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https://nasplib.isofts.kiev.ua/handle/123456789/106997 |
| citation_txt |
Microstructure Investigation of the Spark Plasma Sintered Cu—Al—Ni Shape Memory Material / G.E. Monastyrsky, A.V. Kotko, A.V. Gilchuk, P. Ochin, V.I Kolomytsev., Yu.N. Koval // Металлофизика и новейшие технологии. — 2014. — Т. 36, № 8. — С. 1091-1099. — Бібліогр.: 18 назв. — англ. |
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2025-11-26T18:51:29Z |
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| fulltext |
1091
PACS numbers: 81.05.Bx, 81.07.Bc, 81.07.Wx, 81.20.Ev, 81.30.Kf, 81.30.Mh
Microstructure Investigation of the Spark Plasma Sintered
Cu—Al—Ni Shape Memory Material
G. E. Monastyrsky*,**, A. V. Kotko***, A. V. Gilchuk*, P. Ochin****,
V. I. Kolomytsev**, and Yu. N. Koval**
*National Technical University of Ukraine ‘Kyiv Polytechnic Institute’,
37 Peremogy Prospekt,
UA-03506 Kyiv, Ukraine
**G. V. Kurdyumov Institute for Metal Physics, N.A.S. of Ukraine,
36 Academician Vernadsky Blvd.,
UA-03680 Kyiv-142, Ukraine
***I. M. Frantsevich Institute for Materials Science, N.A.S. of Ukraine,
3 Krzhizhanovskyi Str.,
UA-03680 Kyiv-142, Ukraine
****Institut de Chimie et des Matériaux Paris Est (ICMPE—CNRS),
2—8 Henri Dunant Rue,
94320 Thiais, France
The microstructure of Cu—13.0Al—3.9Ni—0.4Ti—0.2Cr wt.% compacts sin-
tered by spark plasma method from powders prepared by spark-erosion meth-
od in liquid argon from master alloy is investigated. Powder is annealed in H2
atmosphere before the spark plasma sintering. SEM and TEM investigations
reveal that sintered samples have a composite structure, which consists of
the micron and submicron spherical metallic particles embedded into the
binder matrix. This matrix seems to be the product of copper oxide reduction
according to the scheme CuO Cu4O3 Cu2O Cu8O and aluminium hy-
droxides’ conversion according to the flowchart aluminium hydroxide
transition alumina -Al2O3, during the annealing and/or sintering. TEM
study reveals that main phase in metallic particles is self-accommodated 18R
martensite. The regular basal plane stacking faults and/or (001)18R microt-
wins are dominant defects in 18R martensite. 18R martensite of single orien-
tation occupies entire volume of spherical nanoparticles, being the basal
plane stacking faults and/or (001)18R microtwins, which have different
thicknesses.
Досліджено мікроструктуру компактів Cu—13,0Al—3,9Ni—0,4Ti—0,2Cr
ваг.% спечених плазмово-іскровим методом із електроерозійних порош-
ків, виготовлених із мастер-стопу в рідкому арґоні. Перед спіканням по-
Металлофиз. новейшие технол. / Metallofiz. Noveishie Tekhnol.
2014, т. 36, № 8, сс. 1091—1099
Оттиски доступны непосредственно от издателя
Фотокопирование разрешено только
в соответствии с лицензией
2014 ИМФ (Институт металлофизики
им. Г. В. Курдюмова НАН Украины)
Напечатано в Украине.
1092 G. E. MONASTYRSKY, A. V. KOTKO, A. V. GILCHUK et al.
рошок відпалювався в атмосфері водню. Спечені зразки мають композит-
ну структуру, що утворена із мікронних і субмікронних сферичних мета-
левих частинок, вбудованих у зв’язувальну матрицю. Остання є резуль-
татом відновлення під час відпалу та/або спікання оксиду міді відповідно
до схеми CuO Cu4O3 Cu2O Cu8O та гідроксидів алюмінію згідно зі
схемою гідроксид алюмінію перехідний окис алюмінію -Al2O3.
Встановлено, що основною фазою в металевих частинках є самоузгодже-
ний багатоваріянтний 18R-мартенсит, домінантні дефекти якого є реґу-
лярними дефектами пакування в базовій площині та/або (001)18R-
мікродвійники. Весь об’єм сферичних наночастинок займає одноваріянт-
ний 18R-мартенсит; при цьому дефекти пакування в базовій площині
та/або (001)18R-мікродвійники мають різні товщини.
Исследована микроструктура компактов Cu—13,0Al—3,9Ni—0,4Ti—0,2Cr
масс.%, спечённых плазменно-искровым методом из электроэрозионных
порошков, изготовленных из мастер-сплава в жидком аргоне. Перед спе-
канием порошок отжигался в атмосфере водорода. Спечённые образцы
имеют композитную структуру, которая состоит из микронных и субмик-
ронных сферических металлических частиц, встроенных в связующую
матрицу. Последняя является результатом восстановления при отжиге
и/или спекании оксида меди согласно схеме CuO Cu4O3 Cu2O Cu8O
и гидроксидов алюминия согласно схеме гидроксид алюминия пере-
ходный оксид алюминия -Al2O3. Установлено, что основной фазой в
металлических частицах является самосогласованный многовариантный
18R-мартенсит, доминантными дефектами которого являются регуляр-
ные дефекты упаковки в базовой плоскости и/или (001)18R-микро-
двойники. Весь объём сферических наночастиц занимает одновариант-
ный 18R-мартенсит; при этом дефекты упаковки в базовой плоскости
и/или (001)18R-микродвойники имеют разные толщины.
Key words: 18R martensite, basal plane stacking faults, microtwins, Cu—Al—
Ni alloys, spark plasma sintering method, spark-erosion method.
(Received November 28, 2013; in final version, July 07, 2014)
1. INTRODUCTION
Cu—Al—Ni alloys are being developed as ones of the alternatives for the
intermediate temperature application. Polycrystalline Cu—Al—Ni al-
loys produced by conventional casting method are quite brittle [1], due
to their very high elastic anisotropy (A 13), large grain size and
strong orientation dependence of transformation strain [2, 3]. Among
other methods, which refine the substructure, the powder metallurgy
route is a good alternative for near-net shape alloy products with a bet-
ter control of the grain sizes.
The operation with pre-alloyed powders has an unambiguous feed-
back caused by the solid-state diffusion mechanism of powder sinter-
ing. The processes of the decomposition, precipitating and ordering
MICROSTRUCTURE INVESTIGATION OF THE SPARK PLASMA SINTERED Cu—Al—Ni 1093
superimposing on the sintering processes can modify the characteris-
tics of the martensitic transformation (MT). Therefore, the spark
plasma sintering (SPS) method looks as a promising one-step process
alternative to the conventional sintering of pre-alloyed powders. In
our previous work [4], massive Cu—13.01Al—3.91Ni—0.37Ti—0.24Cr
wt.% shape memory alloy was synthesized by the spark plasma sinter-
ing method from pre-alloyed powder prepared by the spark-erosion
method (SE) in liquid argon. XRD, EDS, Auger microanalyses showed
that the composite structure of spark-plasma sintered compacts ap-
pears due to the interaction between Al and CuO oxide from superficial
layers of submicron particles as well as nanofractions of powder. It
could cause the reduction of CuO oxide to Cu2O oxide and promote good
sintering of material even at low temperature of sintering. In addition,
the martensitic phase in the sintered compacts has been clearly indi-
cated by SEM and XRD study. However, smallest scales of the micro-
structure of sintered compacts are not studied.
The aim of current work is to elucidate the peculiarities of micro-
structure of the spark-plasma sintered composite and to reveal the
martensite microstructure of Cu—Al—Ni particles of different scales
embedded in extrinsic matrix.
2. EXPERIMENTAL
Hot-rolled rods of Cu—13.01Al—3.91Ni—0.37Ti—0.24Cr wt.% were
produced by AMT (Belgium). The rods were annealed 30 min at 800C
followed by water quenching. Part of the rods were used as electrodes
for SE apparatus and the remaining were broken in 3—4 mm pieces and
were used to obtain powder by spark erosion method. The general prin-
ciple of the spark-erosion processing is described in details in [5].
The SPS apparatus DR.SINTER® LAB Series is used for sintering.
Uniaxial pressure of maximum 99.5 MPa is applied for densification.
About 1 g of powder was preliminary slightly compacted in the die,
placed inside the working chamber and the system was evacuated. As a
result, the compacts with a diameter of 8 mm and height of 4—6 mm
were obtained.
XRD study of the powder and compacts is carried out at room tem-
perature in Bragg—Brentano configuration with a CoK1,2-radiation. A
PANalyticalX’Pert PRO diffractometer with a linear detector is used.
The morphology and composition study of the sintered samples is ana-
lysed by JSM-6490LV or Auger spectrometer JAMP-9500F both
equipped with EDX spectrometer INCA PentaFETx3. Specimens are
etched by Ar
ions before the inspection. TEM investigation is carried
out with JEOL 100CX operating under accelerating voltage 100 kV.
Samples for the TEM investigation are prepared by the dimpling of 3
mm diameter specimens followed by Ar
ions etching.
1094 G. E. MONASTYRSKY, A. V. KOTKO, A. V. GILCHUK et al.
3. RESULTS AND DISCUSSION
3.1. Phase Content and Microstructure of Sintered Samples
XRD patterns (Fig. 1, a) have shown that, as-obtained powder contains
mainly 3 (L21) phase, (2H) martensite phase, copper oxide CuO (ten-
orite); one minute peak can be attributed to Cu. The width of CuO
peaks is large, thus one can assume that they relate with the nanopar-
ticles of CuO, which appeared due to the reaction with residue of oxy-
gen in liquid argon as well as during the storage. After annealing in
hydrogen, CuO peaks have disappeared completely, instead of them
peaks of Cu2O (ISCD # 75-1531, cuprite) have appeared. In addition,
distinct peaks of 2 (Cu9Al4) were found. After spark plasma sintering
processing, the intensity of 3 and 2 peaks as well as those of marten-
site has diminished dramatically; instead of them peaks of (18R)
phase have appeared.
SEM investigation revealed that after the sintering of spark erosion
powder annealed in H2 atmosphere, the structure is a composite (Fig.
1, b). It consists of the micron and submicron metallic spherical parti-
cles with the compositions close to the master alloys. They are embed-
ded into the matrix, which seems to be mixture of Al and Cu oxides de-
rived from the nanofraction of spark erosion powder. This result has
been already reported elsewhere in details [4, 6].
SEM examinations of Ar
ions etched samples revealed also that
boundaries of the particles as well as interspacing between them (bind-
er fraction) were less etched in comparison with the body of metallic
particles. As a result, the etched particles look as decorated by thin
perhaps ceramic walls.
Fig. 1. a–XRD spectra of as received powder (1), powder annealed in H2 at
290C for 1 hour (2), spark plasma sintered sample (3); b–SEM of Ar
ion
etched spark plasma sintered sample.
MICROSTRUCTURE INVESTIGATION OF THE SPARK PLASMA SINTERED Cu—Al—Ni 1095
3.2. Chemical Composition and Structure of the Binder (Ceramic)
Fraction
TEM investigation has confirmed that the binder fraction that fills the
interspaces between the spherical micron-size particles is the complex
mixture of the oxides. The diffusive and spotted rings, which appeared
on the electron-diffraction patterns taken from different loci of the
samples, indicate the different sizes of the binder components (Fig. 2).
Some of them clearly appeared on the SAED taken from the segments
of the rings (Fig. 2). The surface layer on the micron sized particles
with the typical width 10—30 nm is clearly seen too on dark field imag-
es (Fig. 2). It gives evidence that this layer is also some kind of oxides.
The calculated interplanar spacings are grouped in several clusters,
only five of them are presented on all patterns; others appear only on
certain electron-diffraction patterns. Moreover, the interplanar spac-
ings inside each of groups are slightly different, but these differences
are out of the instrumental error. All this points out that structure of
the binder phase is inhomogeneous and consists of the different kinds
of oxides.
Among the possible candidates, the following is the most relevant as
regards the relative intensity of the reflexes. There are the sets of cop-
per oxides: cuprite Cu2O with cubic symmetry (space group 3Pn m ),
paramelaconite Cu4O3 [7] with tetragonal symmetry (group I41/amd),
and possible one of the cooper suboxides Cu8O [8] with orthorhombic
symmetry (space group Bmm2). Although some of the reflexes on the
rings are well fitted by the reflexes of the monoclinic CuO (tenorite),
its presence in the binder is unlikely, as its strongest reflexes are not
found. Other set of oxides are the aluminium oxides. Except the stable
-Al2O3 (corundum), most of the transition aluminas [9] cannot be ex-
cluded. Some of them with cubic symmetry are preferable since specif-
Fig. 2. Microstructure of the binding fraction. a–diffraction pattern, circle
indicates the area on the ring, from where the DF image was made; b–DF im-
age of the binding fraction. Arrow indicates the interfacial layer on the mi-
cron sized particle with martensite plates inside.
1096 G. E. MONASTYRSKY, A. V. KOTKO, A. V. GILCHUK et al.
ic relations between the interplanar spacing have been observed.
Namely, -alumina [9], -alumina [9, 10] with the composition Al2.67O4
(other name -alumina with spinel-type structure and composition
close to Al2.667O4 [11]), -alumina with the composition close to the
stoichiometric Al21.333O32 [9, 12] both belonging to the space group
3Fd m . Finally, the reflexes of copper—nickel aluminates spinel [13]
CuxNi1—xAl2O4 (space group 3Fd m ) also good fit the spots on the rings.
3.3. Binder Fraction Formation Mechanism
In spite of the lack of certainty in the phase composition of the binder
as well as the interfacial layer of particles, the above-proposed sets of
oxides are plausible. These collections seem to be the result of feasible
scenarios of the transformations between the different type of oxides
and Cu—Al—Ni particles during the preliminary ageing followed by
spark plasma sintering. To explain the transformation of CuO oxide
into Cu2O oxide and large heat release, which has been observed at
900C during the heating of powder, the redox reactions between the
CuO oxide and Al in as-prepared powder has been proposed in [4, 6].
Current TEM investigation has shown that there are several scenarios
of such transformations, which could be fulfilled during the heat
treatments of powder.
The scheme of copper oxide reduction is the following: CuO Cu4O3
Cu2O Cu8O Cu. It seems that the last stage in this chain is ab-
sent. The metastable suboxide Cu8O has the unit-cell volume approxi-
mately four times larger than that of Cu20 and it is usually formed on
early stage of copper oxidation [8]. However, one cannot exclude the
reverse transformation under appropriate conditions, namely the heat-
ing in reduction atmosphere (H2) or in the presence of the elements
with greater affinity to oxygen like aluminium. According to [7], the
Cu4O3 paramelaconit structure can be described either as derived from
the CuO structure by ordered removal of oxygen atoms, or as derived
from the Cu2O structure by ordered insertion of oxygen atom. Thus,
this is the intermediate form between tenorite and cuprite. The reduc-
tion of initial form of copper oxide is terminated on the different steps
of the above-mentioned sequence, depending on the local surrounding
and other conditions affecting the oxygen transport.
According to Ellingham diagram, the reduction of tenorite in hy-
drogen atmosphere has been favourable energetically, independently
on the temperature. On the other hand, the Al presence enhances this
process owing the movement of oxygen atoms from copper oxides to-
ward the aluminium atoms, which have bigger affinity to oxygen. Al-
uminium atoms are present in the powder in two fractions: in
nanofraction, which is formed due to the condensation of vapour phase
during spark erosion, and in the micron-size Cu—Al—Ni particles.
MICROSTRUCTURE INVESTIGATION OF THE SPARK PLASMA SINTERED Cu—Al—Ni 1097
It is hard to believe that aluminium exists in oxygen-free state in
nanofraction due to high affinity of aluminium to oxygen. It also has
not been found in state of suboxide AlO and Al2O [14]. More plausible
that aluminium appears in the nanofraction in various forms of alu-
minium trihydroxides Al(OH)3 (gibbsite, bayerite, nordstrandite)
and/or aluminium oxide hydroxides AlO(OH) (boehmite, diaspore).
These hydroxides are converted during the annealing and/or sintering
into various forms of alumina according to the flowchart: aluminium
hydroxide transition aluminas -Al203 [15]. According to the
flowchart [15], in the temperature interval between 300 and 700C, the
most likely outcome is the transformations into -, - and -alumina
depending on the initial forms of hydroxides and temperature.
There is another attractor for the oxygen atoms, namely, aluminium
atoms on the surface of micron-size particles. Naturally, in that case
the copper—nickel aluminate spinel CuxNi1xAl2O4, which is isomor-
phous to the -, - and -alumina, and have similar lattice parameter is
formed on the surface of Cu—Al—Ni particles during the heat treat-
ments.
3.4. Microstructure of the Micron-, Submicron- and Nanoparticles
TEM investigation of metallic spherical particles reveals several pecu-
liarities. All particles embedded in ceramic binding phase are in mar-
tensite state, at least those ones with the dimension more than 100 nm.
That fact is easily manifested under appropriate conditions such as
needle-like or banded structures inside the particles. Only submicron
and nanosize particles appear as the disks decorated by superficial lay-
er. Larger ones look as grains with irregular curved boundaries that
seem to be related to nonuniform conditions during the Ar
etching.
The self-accommodated 18R martensite plates in (128) twin related
orientations, which occupy the relatively large particle (of size about 1
m) with irregular boundaries, are shown in Fig. 3. The microstruc-
Fig. 3. Microstructure of 18R martensite in the micron sized particle. Dif-
fraction pattern is presented on inset. Zone axis is [210]. BF image (a); DF im-
age (b). Circle indicates the spot, from where the DF image is taken.
1098 G. E. MONASTYRSKY, A. V. KOTKO, A. V. GILCHUK et al.
ture of those crystals consists of typical for Cu—Al—Ni basal plane
stacking faults. Somewhere, the (001) 18R microtwins have been ob-
served. This observation well correlates with the HRTEM investiga-
tion of 18R martensite in Cu—Al alloy [16]. The neighbouring practi-
cally spherical particles sized 300 nm are out of good diffraction condi-
tions.
It is interesting that the smallest particles sized 100—200 nm appear
with striped contrast (Fig. 4, a). It supposed that martensite of only
one variant occupies entire volume of nanosize particle. Because of
their small dimension and adjacent particles in other orientations, it is
very difficult to get good diffraction pattern as well as SAED to reveal
the microstructure of such kind of particles. The rare event under
more or less suitable experimental conditions is presented in Fig. 4, b.
The nanosize particles with (001) 18R microtwins or basal plane stack-
ing faults occupy entire volume of particles; no martensite plates or
accommodation groups of martensite are seen. Similar microstructure
of martensite has be observed by T. Waitz et al. [17] in nanosize grains
after isothermal annealing of high-pressure torsion deformed amor-
phous Ni—50.3 at.% Ti as well as in NiTi nanocrystals embedded into
the amorphous matrix [18]. Other peculiarity is that the width of mi-
crotwins (or stacking faults) is different and their appearing is irregu-
lar.
4. CONCLUSIONS
The microstructure of SPS Cu—13.0Al—3.9Ni—0.4Ti—0.2Cr wt.% com-
pacts sintered from the SE powders prepared in liquid argon consists of
the micron and submicron spherical metallic particles embedded into
the binder matrix. This matrix can be considered as the product of cop-
per oxide reduction (CuO Cu4O3 Cu2O Cu8O) and aluminium hy-
Fig. 4. Microstructure of the smallest particles. a–micron sized and two na-
nosize particles. Calliper indicates the superficial layer on large particle. Ar-
rows indicate the strip contrast in smallest particles; b–BF image of the na-
nosize particle. Diffraction pattern is presented on inset. Zone axis is approx-
imately [210].
MICROSTRUCTURE INVESTIGATION OF THE SPARK PLASMA SINTERED Cu—Al—Ni 1099
droxides conversion (aluminium hydroxide transition aluminas
-Al2O3) during the annealing in H2 atmosphere and/or sintering. The
superficial layer in metallic powder seems to be the copper—nickel alu-
minates spinel CuxNi1xAl2O4. Basic phase in metallic particles is 18R
martensite. The dominant defects are the regular basal plane stacking
faults and/or (001) 18R microtwins. 18R martensite of single orienta-
tion occupies entire volume of spherical nanoparticles, being the basal
plane stacking faults and/or (001) 18R microtwins, which have differ-
ent thicknesses.
ACKNOWLEDGEMENTS
Authors appreciate Prof. G. S. Oliynyk for the consultation and assis-
tance in the Ar
ions etching of the SPS samples for TEM investigation.
REFERENCES
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/NLD (Gebruik deze instellingen om Adobe PDF-documenten te maken die zijn geoptimaliseerd voor prepress-afdrukken van hoge kwaliteit. De gemaakte PDF-documenten kunnen worden geopend met Acrobat en Adobe Reader 5.0 en hoger.)
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/ENU (Use these settings to create Adobe PDF documents best suited for high-quality prepress printing. Created PDF documents can be opened with Acrobat and Adobe Reader 5.0 and later.)
>>
/Namespace [
(Adobe)
(Common)
(1.0)
]
/OtherNamespaces [
<<
/AsReaderSpreads false
/CropImagesToFrames true
/ErrorControl /WarnAndContinue
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/IncludeNonPrinting false
/IncludeSlug false
/Namespace [
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(InDesign)
(4.0)
]
/OmitPlacedBitmaps false
/OmitPlacedEPS false
/OmitPlacedPDF false
/SimulateOverprint /Legacy
>>
<<
/AddBleedMarks false
/AddColorBars false
/AddCropMarks false
/AddPageInfo false
/AddRegMarks false
/ConvertColors /ConvertToCMYK
/DestinationProfileName ()
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/Downsample16BitImages true
/FlattenerPreset <<
/PresetSelector /MediumResolution
>>
/FormElements false
/GenerateStructure false
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/MultimediaHandling /UseObjectSettings
/Namespace [
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(CreativeSuite)
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]
/PDFXOutputIntentProfileSelector /DocumentCMYK
/PreserveEditing true
/UntaggedCMYKHandling /LeaveUntagged
/UntaggedRGBHandling /UseDocumentProfile
/UseDocumentBleed false
>>
]
>> setdistillerparams
<<
/HWResolution [2400 2400]
/PageSize [612.000 792.000]
>> setpagedevice
|