Bulk transport paths through defects in floating zone and Al flux grown SmB$_6$
Yun Suk Eo, Alexa Rakoski, Shriya Sinha, Dmitri Mihaliov, Wesley T. Fuhrman, Shanta R. Saha, Priscila F. S. Rosa, Zachary Fisk, Monica Ciomaga Hatnean, Geetha B… 展开作者
Yun Suk Eo, Alexa Rakoski, Shriya Sinha, Dmitri Mihaliov, Wesley T. Fuhrman, Shanta R. Saha, Priscila F. S. Rosa, Zachary Fisk, Monica Ciomaga Hatnean, Geetha Balakrishnan, Juan R. Chamorro, Seyed M. Koohpayeh, Tyrel M. McQueen, Boyoun Kang, Myung-suk Song, Beongki Cho, Michael S. Fuhrer, Johnpierre Paglione, Cagliyan Kurdak
We investigate the roles of disorder on low-temperature transport in SmB$_6$ crystals grown by both the Al flux and floating zone methods. We used the inverted resistance method with Corbino geometry to investigate whether low-temperature variations in the standard resistance plateau arises from a surface or a bulk channel in floating zone samples. The results show significant sample-dependent residual bulk conduction, in contrast to smaller amounts of residual bulk conduction previously observed in Al flux grown samples with Sm vacancies. We consider hopping in an activated impurity band as a possible source for the observed bulk conduction, but it is unlikely that the large residual bulk conduction seen in floating zone samples is solely due to Sm vacancies. We therefore propose that one-dimensional defects, or dislocations, contribute as well. Using chemical etching, we find evidence for dislocations in both flux and floating zone samples, with higher dislocation density in floating zone samples than in Al flux grown samples. In addition to the possibility of transport through one-dimensional dislocations, we also discuss our results in the context of recent theoretical models of SmB$_6$.
Recent theoretical and experimental findings suggest that the long-known but not well understood low temperature resistance plateau of SmB6 may originate from protected surface states arising from a topologically non-trivial bulk band structure having strong Kondo hybridization. Yet other studies have ascribed this feature to impurity phases, sample vacancies, and surface reconstructions. Given the typical methods used to prepare SmB6 single crystals, the flux and floating zone procedures, these ascriptions should not be taken lightly. Here, we demonstrate how compositional variations and obse…
SmB6 is a candidate topological Kondo insulator that displays surface conduction at low temperatures. Here, we perform torque magnetization measurements as a means to detect de Haas-van Alphen (dHvA) oscillations in SmB6 crystals grown by aluminum flux. We find that dHvA oscillations occur in single crystals containing embedded aluminum, originating from the flux used to synthesize SmB6. Measurements on a sample with multiple, unconnected aluminum inclusions show that aluminum crystallizes in a preferred orientation within the SmB6 cubic lattice. The presence of aluminum is confirmed through b…
The finding of bulk quantum oscillations in the bulk Kondo insulator SmB$_6$, which has been proposed to be a correlated topological insulator, proved a considerable surprise. The subsequent measurement of bulk quantum oscillations in other correlated insulators including YbB$_{12}$ have lent support to our discovery of a class of unconventional insulators that are host to bulk quantum oscillations, of which SmB$_6$ was the first example. Here we perform a series of experiments to examine evidence for the intrinsic character of bulk quantum oscillations in floating zone-grown single crystals o…
High purity Na0.75CoO2 single crystals have been grown by floating zone method. We found the rotation of feed and seed rods play a crucial role in growing high quality single crystal. Systematic investigations suggest the occurrence of a phase separation at microscopic level, such as the separation into Na-rich and Na-poor domains during the growth, and formation of impurity phase(s) depending on growth conditions. NaxCoO2 (x = 0.30, 0.60) crystals have been prepared by sodium deintercalation from Na0.75CoO2. Powder X-ray and energy dispersive X-ray analyses have confirmed the phase purity and…
We have grown La$_{1.37}$Sr$_{1.63}$Mn$_2$O$_7$ single crystals with a laser-diode-heated floating-zone furnace and studied the crystallinity, structure, and magnetoresistance (MR) effect by in-house X-ray Laue diffraction, X-ray powder diffraction, and resistance measurements. The La$_{1.37}$Sr$_{1.63}$Mn$_2$O$_7$ single crystal crystallizes into a tetragonal structure with space group \emph{I}4{/}\emph{mmm} at room temperature. At 0 T, the maximum resistance centers around $\sim$166.9 K. Below $\sim$35.8 K, it displays an insulating character with an increase in resistance upon cooling. An a…
Recent neutron scattering and specific heat studies on the pyrochlore Yb2Ti2O7 have revealed variations in its magnetic behavior below 265mK. In the best samples, a sharp anomaly in the specific heat is observed at T=265mK. Other samples, especially single crystals, have broad features in the specific heat which vary in sharpness and temperature depending on the sample, indicating that the magnetic ground state may be qualitatively different in such samples. We performed detailed comparisons of the chemical structure of a pulverised single crystal of Yb2Ti2O7, grown by the floating zone techni…
A parent insulator of the Bi-based high-$T_c$ superconductor Bi$_2$Sr$_{2-x}$La$_x$CaCu$_2$O$_{8+δ}$ was successfully grown by a traveling solvent floating zone method. The in-plane resistivity $ρ_{ab}$ shows metallic behavior ($dρ_{ab}/dT >$ 0) near room temperature, although the magnitude of the resistivity is far above the Mott limit for metallic conduction. The Hall mobility of the parent insulator does not so much differ from that of an optimally doped sample. These results suggest that the system is not a simple insulator with a well-defined gap, and the hole in the parent insulator is e…
A parent insulator of the Bi-based high-$T_c$ superconductor Bi$_2$Sr$_{2-x}$La$_x$CaCu$_2$O$_{8+δ}$ was successfully grown by a traveling solvent floating zone method. The in-plane resistivity $ρ_{ab}$ shows metallic behavior ($dρ_{ab}/dT >$ 0) near room temperature, although the magnitude of the resistivity is far above the Mott limit for metallic conduction. The Hall mobility of the parent insulator does not so much differ from that of an optimally doped sample. These results suggest that the system is not a simple insulator with a well-defined gap, and the hole in the parent insulator is e…
SrRuO3 is a highly interesting material due to its anomalous-metal properties related with ferromagnetism and its relevance as conductive perovskite layer or substrate in heterostructure devices. We have used optical floating zone technique in an infrared image furnace to grow large single crystals of SrRuO3 with volumes attaining several hundred mm3. Crystals obtained for optimized growth parameters exhibit a high ferromagnetic Curie temperature of 165 K and a low-temperature magnetization of 1.6 muB at a magnetic field of 6 T. The high quality of the crystals is further documented by large r…
We report the optimized conditions for growing the high quality single crystals of candidate quantum spin-ice Pr2Hf2O7 using the optical floating-zone method. Large single crystals of Pr2Hf2O7 have been grown under different growth conditions using a four-mirror type optical floating-zone furnace and their microscopic structural differences have been probed by high-resolution synchrotron x-ray diffraction (SXRD). The SXRD data reveal that the crystals grown under fowing argon (~ 2 L/h) atmosphere with slightly off-stoichiometric (optimized) starting composition yields the highest quality cryst…
We used the inverted resistance method to extend the bulk resistivity of SmB$_{6}$ to a regime where the surface conduction overwhelms the bulk. Remarkably, the bulk resistivity shows an intrinsic thermally activated behavior that changes ten orders of magnitude, suggesting that it is an ideal insulator that is immune to disorder. Non-stoichiometrically-grown SmB$_{6}$ samples also show an almost identical thermally activated behavior. At low temperatures, however, these samples show a mysterious high bulk resistivity plateau, which may arise from extended defect conduction in a 3D TI.
We report on the crystal growth of the quasi one-dimensional quantum spin chain compound SrCuO$_{2}$ and its doped variants containing magnetic cobalt (0.25%, 0.5%, 1% and 2.5%) and non-magnetic zinc (0.5\% and 1\%) impurities. Crystals are grown using the travelling solvent floating zone (TSFZ) method in a four-mirror optical furnace. Some crucial factors, key to the stability of a TSFZ process, including the choice of solvent composition and its associated melting behavior, are discussed in detail. The grown crystals were characterized using x-ray powder diffraction, scanning electron micros…
We report the growth of large single-crystals of Cu2MnAl, a ferromagnetic Heusler compound suitable for polarizing neutron monochromators, by means of optical floating zone under ultra-high vacuum compatible conditions. Unlike Bridgman or Czochralsky grown Cu2MnAl, our floating zone grown single-crystals show highly reproducible magnetic properties and an excellent crystal quality with a narrow and homogeneous mosaic spread as examined by neutron diffraction. An investigation of the polarizing properties in neutron scattering suggests a high polarization efficiency, limited by the relatively s…
The Kondo insulator SmB$_6$ has long been known to display anomalous transport behavior at low temperatures, T$<5$ K. In this temperatures range, a plateau is observed in the dc resistivity, contrary to the exponential divergence expected for a gapped system. Recent theoretical calculations suggest that SmB$_6$ may be the first topological Kondo insulator (TKI) and propose that the residual conductivity is due to topological surface states which reside within the Kondo gap. Since the TKI prediction many experiments have claimed to observe high mobility surface states within a perfectly insulat…
A floating zone furnace is a powerful tool for single crystal growth. Here, we report the floating zone furnace using a high power diode laser of 1kW composed of five 200 Watt heating beams. The five beams with the designed irradiation intensity distribution enable the melt-growth of single crystals for refractory materials having a high melting temperature above 2000°C, volatile materials and even incongruent materials. The power of five beams in the horizontal plane provides uniform intensity in the outer circumference of the raw material rods, while the vertical direction power of five beam…
A series of Yb2Ti2O7 doped samples demonstrates the effects of off-stoichiometry on Yb2Ti2O7's structure, properties, and magnetic ground state via x-ray diffraction, specific heat, and magnetization measurements. A stoichiometric single crystal of Yb2Ti2O7 grown by the traveling solvent floating zone technique (solvent = 30 wt% rutile TiO2 and 70 wt% Yb2Ti2O7) is characterized and evaluated in light of this series. Our data shows that upon positive x doping, the cubic lattice parameter a increases and the Curie-Weiss temperature decreases. Heat capacity measurements of stoichiometric Yb2Ti2O7…
We report a study on the crystal growth of the hexagonal manganites $R$MnO$_3$ ($R$ = Y, Lu, Ho, Er, and Tm) by using an optical floating-zone method. It was found that high-quality single crystals of $R$ = Y, Lu, and Ho could be easily grown with essentially the same conditions as those reported in literature, that is, with an atmosphere of normal pressure Ar and oxygen mixture and a growth rate of 2--4 mm/h. However, these conditions were not feasible for growing good crystals of $R$ = Er and Tm. The chemical analysis indicated that it was due to an off-stoichiometric phenomenon in the forme…
This study reports atomic-scale characterization of structural defects in Yb2Ti2O7, a pyrochlore oxide whose subtle magnetic interactions is prone to small perturbations. Due to discrepancies in the reported magnetic ground states, it has become a pressing issue to determine the nature of defects in this system. In the present study, we use atomic resolution scanning transmission electron microscopy techniques to identify the type of defects in the ytterbium titanate single crystals grown by the conventional optical floating zone (FZ) method. In addition to the known point defects of substitut…
Single crystals of PrNiO3 were grown under an oxygen pressure of 295 bar using a unique high-pressure optical-image floating zone furnace. The crystals, with volume in excess of 1 mm3, were characterized structurally using single crystal and powder X-ray diffraction. Resistivity, specific heat, and magnetic susceptibility were measured, all of which evidenced an abrupt, first order metal-insulator transition (MIT) at ~130 K, in agreement with previous literature reports on polycrystalline specimens. Temperature-dependent single crystal diffraction was performed to investigate changes through t…
Mm-sized LiMn$_{1-x}$Fe$_x$PO$_4$ single crystals with $0\leq x \leq 1$ were grown by means of the traveling floating-zone technique at elevated Argon pressure of 30~bar. For the various doping levels, the growth process was optimized with respect to the composition-dependant effective light absorption and transparency of the materials. A convex crystal/melt interface, determined by the angle of incident light, was identified to be particularly crucial for a successful growth. The resulting large single crystalline grains are stoichiometric. Structure refinement shows that lattice parameters a…
The wealth of structural phases seen in the rare-earth disilicate compounds promises an equally rich range of interesting magnetic properties. We report on the crystal growth by the optical floating zone method of members of the rare-earth disilicate family, $R_{2}$Si$_{2}$O$_{7}$ (with $R=$ Er, Ho, and Tm). Through a systematic study, we have optimised the growth conditions for Er$_{2}$Si$_{2}$O$_{7}$. We have grown, for the first time using the floating zone method, crystal boules of Ho$_{2}$Si$_{2}$O$_{7}$ and Tm$_{2}$Si$_{2}$O$_{7}$ compounds. We show that the difficulties encountered in t…
High quality single crystals of BaFe$_{12}$O$_{19}$ were grown using the floating zone technique in flowing oxygen pressurized to 100 atm. Single crystal neutron diffraction was used to determine the nuclear and magnetic structure of BaFe$_{12}$O$_{19}$ at 4 K and 295 K. At both temperatures, there exist local electric dipoles formed by the off-mirror-plane displacements of magnetic Fe$^{3+}$ ions at the bipyramidal sites. The displacement at 4 K is about half of that at room temperature. The temperature dependence of the specific heat shows no anomaly associated with long range polar ordering…
Single crystals of the metallic Ruddlesden-Popper trilayer nickelates R$_4$Ni$_3$O$_{10}$ (R=La, Pr) were successfully grown using an optical-image floating zone furnace under oxygen pressure (pO$_2$) of 20 bar for La$_4$Ni$_3$O$_{10}$ and 140 bar for Pr$_4$Ni$_3$O$_{10}$. A combination of synchrotron and laboratory x-ray single crystal diffraction, high-resolution synchrotron x-ray powder diffraction and measurements of physical properties revealed that R$_4$Ni$_3$O$_{10}$ (R=La, Pr) crystallizes in the monoclinic $P$2$_1$/$a$ (Z=2) space group at room temperature, and that a metastable ortho…
Temperature and current dependences of resistivity of bulk La$_{0.75}$Ca$_{0.25}$MnO$_{3}$ sample grown by the floating-zone method were studied using single ramp pulses of current. It is found that near the Curie temperature $T_C$ the sample resistance depends substantially on current magnitude. The observed features can be determined by inhomogeneous Joule overheating due to mixed phase state of manganites near the ferromagnetic-paramagnetic transition and percolation character of this transition.
