Effect of temperature and pressure to pinning centers in bulk MgB₂ under high pressure
The MgB₂-based samples were synthesized at 2 GPa at 800 and 1050 °C for 1 hour with and without Ti and SiC. X-ray, SEM and Auger structural studies showed that with increasing of manufacturing temperature grain boundary pinning transforms into point pinning, which is well correlated with the transfo...
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irk-123456789-1196072017-06-08T03:02:33Z Effect of temperature and pressure to pinning centers in bulk MgB₂ under high pressure Kozyrev, A. Международная научно-практическая конференция «Нанотехнологии и наноматериалы» The MgB₂-based samples were synthesized at 2 GPa at 800 and 1050 °C for 1 hour with and without Ti and SiC. X-ray, SEM and Auger structural studies showed that with increasing of manufacturing temperature grain boundary pinning transforms into point pinning, which is well correlated with the transformation of discontinuous oxygen enriched layers into separately located Mg–B–O inclusions in MgB₂. Ti and SiC additions can influence the oxygen and boron distribution, but cannot change the type of pinning at relatively low temperatures. 2014 Article Effect of temperature and pressure to pinning centers in bulk MgB₂ under high pressure / A. Kozyrev // Физика низких температур. — 2014. — Т. 40, № 8. — С. 964-967. — Бібліогр.: 10 назв. — англ. 0132-6414 PACS 74.70.Ad, 74.62.Dh, 74.62.Fj http://dspace.nbuv.gov.ua/handle/123456789/119607 en Физика низких температур Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України |
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Международная научно-практическая конференция «Нанотехнологии и наноматериалы» Международная научно-практическая конференция «Нанотехнологии и наноматериалы» |
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Международная научно-практическая конференция «Нанотехнологии и наноматериалы» Международная научно-практическая конференция «Нанотехнологии и наноматериалы» Kozyrev, A. Effect of temperature and pressure to pinning centers in bulk MgB₂ under high pressure Физика низких температур |
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The MgB₂-based samples were synthesized at 2 GPa at 800 and 1050 °C for 1 hour with and without Ti and SiC. X-ray, SEM and Auger structural studies showed that with increasing of manufacturing temperature grain boundary pinning transforms into point pinning, which is well correlated with the transformation of discontinuous oxygen enriched layers into separately located Mg–B–O inclusions in MgB₂. Ti and SiC additions can influence the oxygen and boron distribution, but cannot change the type of pinning at relatively low temperatures. |
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Kozyrev, A. |
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Kozyrev, A. |
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Kozyrev, A. |
| title |
Effect of temperature and pressure to pinning centers in bulk MgB₂ under high pressure |
| title_short |
Effect of temperature and pressure to pinning centers in bulk MgB₂ under high pressure |
| title_full |
Effect of temperature and pressure to pinning centers in bulk MgB₂ under high pressure |
| title_fullStr |
Effect of temperature and pressure to pinning centers in bulk MgB₂ under high pressure |
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Effect of temperature and pressure to pinning centers in bulk MgB₂ under high pressure |
| title_sort |
effect of temperature and pressure to pinning centers in bulk mgb₂ under high pressure |
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Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України |
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| citation_txt |
Effect of temperature and pressure to pinning centers in bulk MgB₂ under high pressure / A. Kozyrev // Физика низких температур. — 2014. — Т. 40, № 8. — С. 964-967. — Бібліогр.: 10 назв. — англ. |
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Low Temperature Physics/Fizika Nizkikh Temperatur, 2014, v. 40, No. 8, pp. 964–967
Effect of temperature and pressure to pinning centers
in bulk MgB2 under high pressure
A. Kozyrev
Institute for Superhard Materials of the National Academy of Sciences of Ukraine
2 Avtozavodskaya Str., Kiev 07074, Ukraine
E-mail: kozyrev-a@list.ru
Received December 18, 2013, published online June 23, 2014
The MgB2-based samples were synthesized at 2 GPa at 800 and 1050 °C for 1 hour with and without Ti
and SiC. X-ray, SEM and Auger structural studies showed that with increasing of manufacturing temperature
grain boundary pinning transforms into point pinning, which is well correlated with the transformation of dis-
continuous oxygen enriched layers into separately located Mg–B–O inclusions in MgB2. Ti and SiC addi-
tions can influence the oxygen and boron distribution, but cannot change the type of pinning at relatively low
temperatures.
PACS: 74.70.Ad Metals; alloys and binary compounds (including A15, MgB2, etc.);
74.62.Dh Effects of crystal defects, doping and substitution;
74.62.Fj Effects of pressure.
Keywords: superconductivity, magnesium diboride, titanium, silicon carbide, critical current density.
Introduction
The great interest in MgB2-based superconductors is de-
termined by their coherence length (ξab(0) = (3.7–12) nm,
ξc(0) = (1.6–3.6) nm). This value is comparatively large
and allows high critical current flow in polycrystalline
MgB2 through the grain boundaries [1]. It is widely be-
lieved that in MgB2, any inclusions of secondary phases
comparable with the coherence length and grain bounda-
ries themselves [2] can pin nonsuperconducting vortices
leading to a critical current density increase. Up to now
only grain boundary pinning, i.e., pinning of many non-
superconductive vortices along the boundary of grains,
has been observed for MgB2. On the other hand, so-called
point pinning, where only one vortex can be pinned by a
structural defect, was never observed. The upper critical
field Bc2 of MgB2 can be successfully increased by intro-
ducing some disorder into the MgB2 crystal lattice (by
adding carbon, for example), which reduces its anisotro-
py and opens up the possibility to attain higher currents at
high magnetic fields [3].
The improved material performance needs clean grain
boundaries between the MgB2 grains and a good connec-
tivity between them; the latter can be successfully achieved
by manufacturing (synthesis or sintering) under enhanced
or high pressure. A denser material not only exhibits better
superconducting and mechanical properties, which is of
great importance because of the necessity to work in strong
magnetic fields under thermocycling conditions, but also
higher stability against degradation because it reacts less
with moisture and gases.
Several previous investigations have shown that MgB2-
based materials usually contain a high amount of admixed
oxygen in their structure, which does not prevent their ex-
cellent superconducting performance [4–6]. This oxygen
enters in Mg(B,O)2 inclusions, which can be pinning cen-
ters in MgB2 [7].
Our previous study [8] showed that MgB2-based bulk
materials prepared under high pressure had higher criti-
cal current densities in high magnetic fields, when prepara-
tion temperatures were 600–800 °C, and in lower magnetic
fields — when preparation temperatures were 1050 °C. It
has been shown by the authors of paper [8] that increasing
the pressure during manufacturing enhances the volume
pinning force and moves the position of the maximum to
higher magnetic fields. A similar shift was observed, when
Ti or SiC was added. It has been established that tempera-
ture syntheses materials is correlate with volume of pin-
ning and with formation of Mg–B–O oxygen-enriched re-
gions.
© A. Kozyrev, 2014
Effect of temperature and pressure to pinning centers in bulk MgB2 under high pressure
Experiment
The MgB2-based samples were prepared by heating
pre-compacted Mg and B powder mixtures with and with-
out additions of Ti and SiC up to 800–1050 °C under a high
quasi-hydrostatic pressure of 2 GPa in a recessed-anvil-
type high-pressure apparatus. Boron powder with grain
size < 5 μm was used as starting materials. The boron pow-
ders and metal magnesium turnings Mg were mixed and
milled in a high-speed planetary activator with steel balls
for 1–3 min. To investigate the effect of additions, 10 wt%
Ti (grain size 1–3 μm, 99% purity) or SiC (200–800 nm)
were added to the Mg and B powder mixture.
The structure of the materials was examined by x-ray
diffraction (with Rietveld refinement) and by SEM with
microprobe x-ray and Auger (JAMP−9500F) options. The
critical current density was obtained from magnetization
measurements in an Oxford Instruments 3001 vibrating
sample magnetometer (VSM) using the Bean model. The
pinning mechanism was estimated using a method pro-
posed in [9]: k = Bpeak/Bn, where Bpeak is the field, where
the volume pinning force is maximal (Fp(max)) and Bn is
the field, at which Fp(max) drops to half on the high field
side; k is expected to be at 0.34 and 0.47 for grain bounda-
ry (GBP) and point pinning (PP), respectively. Connectivi-
ty, Bc2 and Birr were estimated based on resistivity meas-
urements by the four-probe method (direct current flow
through the materials) in magnetic fields of up to 15 T. The
typical dependence of the critical current densities for the
HP-synthesized materials is shown in Fig. 1.
Results
Figures 2–5 present the microstructure of materials syn-
thesized under high pressure 2 GPa. As can be seen from
the photos, their structure contains dark inclusions of high-
er magnesium borides MgBx (x > 2). For the HP samples,
the stoichiometry of higher borides was usually x > 8–12.
However for the SPS (spark plasma sintering, 50 MPa)
samples, the stoichiometry of higher borides was not high-
er than x = 4–7. Materials synthesized at low temperatures
(800 °C) generally contain a higher amount of higher bo-
rides and the inclusions are coarser. Another type of inclu-
sions observed in the material structures as bright areas.
The composition of these inclusions is close to Mg:B:O in
a ratio 1:0.8:0.9. Probably that they have MgO structure
with embedded B, because the x-ray phase analysis (with
Rietveld refinement) usually shows two phases: MgB2 and
MgO (up to 5–30 wt%).
Higher magnesium borides with x > 4 are not seen in
the x-ray diffraction patterns [5], possibly because their
inclusions are dispersed in the structure and have compli-
cated unit cells with many reflection planes (which makes
the x-ray reflections of higher borides rather weak, looking
like noise on the MgB2 background). SEM and Auger
studies showed some other results that x-ray analysis with
Rietveld refinement. For example MgB2 with high critical
current density synthesized under 2 GPa at temperature
1050 °C (Fig. 3) showed 75 wt% of MgB2 and 25 wt% of
MgO by x-ray, but careful SEM and Auger studies showed
the presence Mg–B–O inclusions with stoichiometry
1 : 0.5–0.8 : 0.8–0.9 and 1 : 11–13 : 0.2–0.5 (close to
MgB12). These inclusions are visible in the image of the
microstructure as small white and black areas. The gray
matrix phase that fills the space between them, has the
stoichiometry 1 : 1.7–2.2 : 0.3–0.6 (close to MgB2). Thus,
some oxygen is present in any point of the sample, but
nevertheless its distribution is not uniform. With increasing
temperature (from 800 to 1050 °C), the number of white
inclusions increases and the boundaries between areas are
becoming sharper.
Figures 2, 3 show the evolution of the oxygen and bo-
ron distribution in the structure of materials prepared
at 2 GPa with the manufacturing temperature from 800
to 1050 °C. With increasing manufacturing temperature
the segregation of admixed oxygen and the formation of
separate oxygen enriched Mg–B–O inclusions are more
pronounced. In the materials prepared at 800 °C the for-
mation of oxygen-enriched Mg–B–O layers (15–30 nm)
were observed. In the materials prepared at 1050 °C local
Mg–B–O inclusions are forming.
The addition of SiC at low processing temperature
(800 °C) also changed the oxygen distribution. So-called
“layered” Mg–B–O structure (Fig. 2) was transformed into
a structure with separate Mg–B–O inclusions (Fig. 4) due
to the addition of SiC. However, this redistribution at
800 °C does not affect the type of pinning.
The increase in the synthesis temperature up to 1050 °C
caused a total change in value of pinning and its type
[10]. In the synthesis of the samples under a pressure of
2 GPa at 1050 °C, the pinning force was 7.6·109 N/m3 for
Fig. 1. Typical dependence of the critical current density at dif-
ferent temperatures on magnetic field for materials synthesized at
2 GPa at 800 °C and 1050 °C for 1 h.
Low Temperature Physics/Fizika Nizkikh Temperatur, 2014, v. 40, No. 8 965
A. Kozyrev
pure MgB2, 10.9·109 N/m3 for MgB2 with addition of
SiC and 4.8·109 N/m3 for MgB2 with addition of Ti. If
the synthesis temperature was 800 °C, the pinning force
was 1.6·109 N/m3 for pure MgB2 and 1.9·109 N/m3 for
MgB2 with addition of SiC and Ti. In the first case there
is a point pinning; in the second — grain boundary pin-
ning. In sample with additions of titanium and tempera-
ture of synthesis 1050 °C is observed a so-called mixed
pinning (something intermediate between the point and
the grain-boundary pinning).So pinning force, as studies
have shown, is highly dependent on the synthesis tempe-
rature.
Fig. 4. The microstructure (SEI and COMPO) of MgB2 materials prepared from Mg:2B mixtures with addition of SiC (10%) at 2 GPa,
800 °C for 1 h.
Fig. 2. The microstructure (SEI and COMPO) of MgB2 materials prepared from Mg:2B mixtures without additions at 2 GPa, 800 °C for
1 h.
Fig. 3. The microstructure (SEI and COMPO) of MgB2 materials prepared from Mg:2B mixtures without additions at 2 GPa, 1050 °C
for 1 h.
966 Low Temperature Physics/Fizika Nizkikh Temperatur, 2014, v. 40, No. 8
Effect of temperature and pressure to pinning centers in bulk MgB2 under high pressure
All materials prepared at 1050 °C demonstrated high
connectivity — 80–87%.
Summary
The effect of temperature on the structure of magnesi-
um diboride synthesizing under 2 GPa is mainly a redistri-
bution of boron and oxygen. With increasing temperature
(from 800 to 1050 °C), the number of inclusions with high
content of oxygen increase and the boundaries between
areas are becoming sharper. Also segregation of admixed
oxygen and the formation of separate oxygen enriched
inclusions occurs. Adding silicon carbide and titanium is
even more prominent, segregation of oxygen and with in-
creasing temperature changes the type of pinning, from
grain boundary to a point pinning.
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1050 °C for 1 h.
Low Temperature Physics/Fizika Nizkikh Temperatur, 2014, v. 40, No. 8 967
http://dx.doi.org/10.1007/s10948-012-2001-7
Introduction
Experiment
Results
Summary
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/ENU (Use these settings to create Adobe PDF documents that are to be checked or must conform to PDF/A-1b, an ISO standard for the long-term preservation \(archival\) of electronic documents. For more information on creating PDF/A compliant PDF documents, please refer to the Acrobat User Guide. Created PDF documents can be opened with Acrobat and Adobe Reader 5.0 and later.)
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>> setdistillerparams
<<
/HWResolution [2400 2400]
/PageSize [612.000 792.000]
>> setpagedevice
|