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We present the refinement of the crystal structure of charge-ordered LuFe2O4, based on single-crystal x-ray diffraction data. The arrangement of the different Fe-valence states, determined with bond-valence-sum analysis, corresponds to a stacking of charged Fe bilayers, in contrast to the polar bilayers previously suggested. This arrangement is supported by an analysis of x-ray magnetic circular dichroism spectra, which also evidences a strong charge-spin coupling. The non-polar bilayers are inconsistent with charge order based ferroelectricity., Comment: 5 pages, 3 figures

We present a detailed study of magnetism in LuFe2O4, combining magnetization measurements with neutron and soft x-ray diffraction. The magnetic phase diagram in the vicinity of T_N involves a metamagnetic transition separating an antiferro- and a ferrimagnetic phase. For both phases the spin structure is refined by neutron diffraction. Observed diffuse magnetic scattering far above T_N is explained in terms of near degeneracy of the magnetic phases., Comment: 5 pages, 5 figures + 6 pages of supplementary information

Nuclear resonant inelastic x-ray scattering on quartz structured 57FePO4 as a function of pressure, up to 8 GPa reveals hardening of the low-energy phonons under applied pressures up to 1.5 GPa, followed by a large softening at 1.8 GPa upon approaching the phase transition pressure of ~2 GPa. The pressure-induced phase transitions in quartz-structured compounds have been predicted to be related to a soft phonon mode at the Brillouin-zone boundary (1/3, 1/3, 0) and to the break-down of the Born-stability criteria. Our results provide the first experimental evidence of this predicted phonon softening., Comment: 6 pages, 4 figures

We investigated the series of temperature and field-driven transitions in LuFe$_2$O$_4$ by optical and M\"{o}ssbauer spectroscopies, magnetization, and x-ray scattering in order to understand the interplay between charge, structure, and magnetism in this multiferroic material. We demonstrate that charge fluctuation has an onset well below the charge ordering transition, supporting the "order by fluctuation" mechanism for the development of charge order superstructure. Bragg splitting and large magneto optical contrast suggest a low temperature monoclinic distortion that can be driven by both temperature and magnetic field., Comment: 4 pages, 3 figures, PRL in print

X-ray scattering by multiferroic LuFe2O4 is reported. Below 320 K, superstructure reflections indicate an incommensurate charge order with propagation close to (1/3,1/3,3/2). The corresponding charge configuration, also found by electronic structure calculations as most stable, contains polar Fe/O double-layers with antiferroelectric stacking. Diffuse scattering at 360 K, with (1/3,1/3,0) propagation, indicates ferroelectric short-range correlations between neighboring double-layers. The temperature dependence of the incommensuration indicates that charge order and magnetism are coupled., Comment: v2: added more details on representation analysis; edited for accessibility to general readership. PRL in print

We present single-crystal neutron diffraction measurements on multiferroic LuFe2O4 showing phase transitions at 240 and 175 K. Magnetic reflections are observed below each transition indicating that the magnetic interactions in LuFe2O4 are 3-dimensional (3D) in character. The magnetic structure is refined as a ferrimagnetic spin configuration below the 240 K transition. While 3D magnetic correlations persists below 175 K, a significant broadening of the magnetic peaks is observed along with the build up of a diffuse component to the magnetic scattering., Comment: 4 figures

The temperature dependence of charge order in Fe2OBO3 was investigated by resistivity and differential scanning calorimetry measurements, Mossbauer spectroscopy, and synchrotron x-ray scattering, revealing an intermediate phase between room temperature and 340 K, characterized by coexisting mobile and immobile carriers, and by incommensurate superstructure modulations with temperature-dependent propagation vector (1/2,0,tau). The incommensurate modulations arise from specific anti-phase boundaries with low energy cost due to geometrical charge frustration., Comment: 4 p., 5 fig.; v2: slightly expanded introduction + minor changes. PRL in print

Solution-grown single crystals of Fe2OBO3 were characterized by specific heat, Mossbauer spectroscopy, and x-ray diffraction. A peak in the specific heat at 340 K indicates the onset of charge order. Evidence for a doubling of the unit cell at low temperature is presented. Combining structural refinement of diffraction data and Mossbauer spectra, domains with diagonal charge order are established. Bond-valence-sum analysis indicates integer valence states of the Fe ions in the charge ordered phase, suggesting Fe2OBO3 is the clearest example of ionic charge order so far., Comment: 4 pages, 5 figures. Fig. 3 is available in higher resolution from the authors. PRL in print

Differential thermal analysis on metallic alloys containing volatile elements can be highly problematic. Here we show how measurements can be performed in commercial, small-sample, equipment without modification. This is achieved by using a sealed Ta crucible, easily fabricated from Ta tubing and sealed in a standard arc furnace. The crucible performance is demonstrated by measurements on a mixture of Mg and MgB$_2$, after heating up to 1470$^{\circ}{\rm C}$. We also show data, measured on an alloy with composition Gd$_{40}$Mg$_{60}$, that clearly shows both the liquidus and a peritectic, and is consistent with published phase diagram data.

To obtain single crystals by solution growth, an exposed primary solidification surface in the appropriate, but often unknown, equilibrium alloy phase diagram is required. Furthermore, an appropriate crucible material is needed, necessary to hold the molten alloy during growth, without being attacked by it. Recently, we have used the comparison of realistic simulations with experimental differential thermal analysis (DTA) curves to address both these problems. We have found: 1) complex DTA curves can be interpreted to determine an appropriate heat treatment and starting composition for solution growth, without having to determine the underlying phase diagrams in detail. 2) DTA can facilitate identification of appropriate crucible materials. DTA can thus be used to make the procedure to obtain single crystals of a desired phase by solution growth more efficient. We will use some of the systems for which we have recently obtained single-crystalline samples using the combination of DTA and solution growth as examples. These systems are TbAl, Pr$_7$Ni$_2$Si$_5$, and YMn$_4$Al$_8$., Comment: 17 pages, 8 figures

Single crystals of flux-grown tetragonal GdFe4Al8 were characterized by thermodynamic, transport, and x-ray resonant magnetic scattering measurements. In addition to antiferromagnetic order at TN ~ 155 K, two low-temperature transitions at T1 ~ 21 K and T2 ~ 27 K were identified. The Fe moments order at TN with an incommensurate propagation vector (tau,tau,0) with tau varying between 0.06 and 0.14 as a function of temperature, and maintain this order over the entire T

Measurements of the superconducting transition temperatures for Al-doped, C-doped and neutron-damaged-annealed MgB2 samples under pressure up to ~8 kbar are presented. The dT_c/dP values change systematically with the decrease of the ambient pressure T_c in a regular fashion. The evolution of the pressure derivatives can be understood assuming that the change in phonon spectrum is a dominant contribution to dT_c/dP.

The temperature dependence of the upper critical field, Hc2, for both field directions in partially substituted polycrystalline MgB2 was determined. Whereas the suppression of Tc is similar for aluminum and carbon substituted samples, Hc2 is affected by the substitution in profoundly different ways. In the case of Al substitution changes can tentatively be described by intrinsic effects (shift of the Fermi level). In the C substituted samples, Hc2 is increased drastically, and extrinsic effects (disorder) have to play a major role. The strong contrast between the two substitutions is discussed, taking into account three relevant scattering rates., Comment: 6 pages, 4 figures

Magnetization and muon spin relaxation on MgB2 were measured as a function of field at 2 K. Both indicate an inverse-squared penetration depth strongly decreasing with increasing field H below about 1 T. Magnetization also suggests the anisotropy of the penetration depth to increase with increasing H, interpolating between a low Hc1 and a high Hc2 anisotropy. Torque vs angle measurements are in agreement with this finding, while also ruling out drastic differences between the mixed state anisotropies of the two basic length scales penetration depth and coherence length., Comment: 4 pages, 4 figures

The upper critical field Hc2||c(0) of 85 kOe in Mg(B0.94C0.06)2 single crystals, determined from torque measurements, is more than twice as large as that one of 31 kOe in unsubstituted MgB2. Anisotropy of Hc2 increases from about 3.4 near Tc, the value close to that in MgB2, to about 4 at low temperature, the value considerably lower than that in MgB2. The corresponding Hc2||ab(0) of about 330-350 kOe is likely close to the maximum enhancement due to C substitution. The position of a sharp peak in the irreversible torque Hmax was found to be shifted to lower reduced fields H/Hc2 in comparison to its position in unsubstituted MgB2, indicating increasing disorder. The enhancement of Hc2 can be explained as a disorder effect only if the main result of disorder is to make the p bands more dirty while not affecting the s bands as much. In addition to disorder and weakened electron-phonon coupling, the impact of the Fermi level shifting into a region with lower s Fermi velocities has to be taken into account in the analysis of Hc2 data as well., Comment: PDF only, 17 pages, 5 figures

We report site-selective oxygen isotope ($^{16}$O/$^{18}$O) effect (OIE) measurements on the in-plane penetration depth $\lambda_{ab} $ in underdoped Y$_{0.6}$Pr$_{0.4}$Ba$_2$Cu$_3$O$_{7-\delta}$, using the muon-spin rotation ($\mu$SR) technique. A pronounced OIE on the transition temperature $T_c$ as well as on $\lambda_{ab}^{-2}(0)$ was observed, which mainly arises from the oxygen sites within the superconducting CuO$_2$ planes (100 % within error bar). The values of the corresponding relative isotope shifts were found to be $T_c/T_c= -3.7(4)%$ and $\Delta\lambda^{-2}_{ab}(0)/\lambda^{-2}_{ab}(0)= -6.2(1.0)%$. Our results imply that in this compound the phonon modes involving the movement of planar oxygen are dominantly coupled to the electrons., Comment: 4pages, 4 figures

The magnetic penetration depth $\lambda(0)$ in polycrystalline MgB$_{2}$ for different boron isotopes ($^{10}$B/$^{11}$B) was investigated by transverse field muon spin rotation. No boron isotope effect on the penetration depth $\lambda(0)$ was found within experimental error: $\Delta\lambda(0)/\lambda(0) = -0.8(8)%$, suggesting that MgB$_{2}$ is an adiabatic superconductor. This is in contrast to the substantial oxygen isotope effect on $\lambda(0)$ observed in cuprate high-temperature superconductors., Comment: 5 pages, 3 figures, 1 table

Magnesium diboride MgB2 has been an extraordinarily hot research topic since the discovery of superconductivity below 40 K, due to the vast amount of unusual properties originating from the involvement in superconductivity of two sets of bands that are of a different dimensionality. We review, with a strong focus on results obtained by torque magnetometry, how this leads to a complex behavior of the anisotropic superconducting state properties. The different dimensionality of the two sets of bands is manifested in the upper critical field Hc2 anisotropy, which was found to strongly decrease with increasing temperature. While the angular dependence of Hc2 follows roughly the predictions of anisotropic Ginzburg-Landau theory AGLT, small, but systematic deviations were observed near Tc. This, and the temperature dependent anisotropy, witness a breakdown of the AGLT description of MgB2, even close to Tc. Theoretical calculations are in qualitative agreement with the observed angle dependence, but suggest a much lower penetration depth anisotropy at low temperatures. Reversible torque vs angle curves in the mixed state indicate that the penetration depth anisotropy in intermediate fields has to be higher than currently available theoretical estimates. The observed field dependent effective anisotropies can be accounted for qualitatively by the faster depression of superconductivity in the more isotropic bands by the applied field. The vortex matter phase diagram is drawn, based on measurements of the reversible and irreversible torque in the mixed state. In the irreversible torque, a peak effect (PE) was observed in fields of about 0.85 Hc2. History effects of the critical current density in the PE region suggest that the PE signifies an order-disorder transition of vortex matter., Comment: 38 pages, 15 figures (4 of them in reduced quality to meet size limitation), review of superconducting state anisotropies and phase diagram, with strong focus on torque results; invited chapter in vol. 1 of 'Horizons in Superconductivity Research' (Nova Publishers, NY), in print; v2 = 1 typo corrected

Single crystals of MgB2 have been grown with a high-pressure cubic anvil technique. They grow via the peritectic decomposition of the MgNB9 ternary nitride. The crystals are of a size up to 2x1x0.1mm3 with a weight up to 230 micrograms. Typically they have transition temperatures between 38 and 38.6 K with a width of 0.3-0.5 K. Investigations of the P-T phase diagram prove that the MgB2 phase is stable at least up to 2190C at high hydrostatic pressure in the presence of Mg vapor under high pressure. Substitution of aluminum for magnesium in single crystals leads to stepwise decrease of Tc. This indicates a possible appearance of superstructures or phases with different Tc's. The upper critical field decreases with Al doping., Comment: 6 pages, 2 figures. submitted to Physica C (M2S-Rio proceedings). Text and Fig.2 revised

Anisotropic properties of superconducting MgB2 obtained by torque magnetometry are compared to theoretical predictions, concentrating on two issues. Firstly, the angular dependence of Hc2 is shown to deviate close to Tc from the dependence assumed by anisotropic Ginzburg-Landau theory. Secondly, from the evaluation of torque vs angle curves it is concluded that the anisotropy of the penetration depth gamma_lambda has to be substantially higher at low temperature than theoretical estimates, at least in fields higher than 0.2 T., Comment: 2 p.,2 Fig., submitted to Physica C (M2S-Rio proceedings); v2: 1 ref added

Single crystals of MgB2 have been grown at high pressure via the peritectic decomposition of MgNB9. The crystals are of a size up to 1.5x0.9x0.2 mm3 with a weight up to 0.23 mg, and typically have transition temperatures between 37 and 39 with a width of 0.3-0.5 K. Investigations of the P-T phase diagram prove that the MgB2 phase is stable at least up to 2190 C at high hydrostatic pressure in the presence of Mg vapor under high pressure. Small variations of Tc are caused by doping with metal elements from the precursor or annealing of defects during the crystal growth process., Comment: PDF only, 12 pages, 4 figures. Physica C (special MgB2 issue) in print (proof available online with ScienceDirect)

The angular and temperature dependence of the upper critical field Hc2 in MgB2 was determined from torque magnetometry measurements on single crystals. The Hc2 anisotropy gamma_H was found to decrease with increasing temperature, in disagreement with the anisotropic Ginzburg-Landau theory, which predicts that the gamma_H is temperature independent. This behaviour can be explained by the two band nature of superconductivity in MgB2. An analysis of measurements of the reversible torque in the mixed state yields a field dependent effective anisotropy gamma_eff, which can be at least partially explained by different anisotropies of the penetration depth and the upper critical field. It is shown that a peak effect in fields of about 0.85 Hc2 is a manifestation of an order-disorder phase transition of vortex matter. The H-T phase diagram of MgB2 for H//c correlates with the intermediate strength of thermal fluctuations in MgB2, as compared to those in high and low Tc superconductors., Comment: 12 pages, 8 figures, Physica C in print (invited paper for a special issue on MgB2)

Single crystals of MgB2 with a size up to 1.5x0.9x0.2 mm3 have been grown with a high pressure cubic anvil technique. The crystal growth process is very peculiar and involves an intermediate nitride, namely MgNB9. Single crystals of BN and MgB2 grow simultaneously by a peritectic decomposition of MgNB9. Magnetic measurements in fields of 1-5 Oe show sharp transitions to the superconducting state at 37-38.6 K with width of ~0.5 K. The high quality of the crystals allowed the accurate determination of magnetic, transport and optical properties as well as scanning tunnelling spectroscopy (STS) and decoration studies. Investigations of crystals with torque magnetometry show that Hc2//c is very low (24 kOe at 15 K), while Hc2//ab increases up to 140 kOe at 15 K. The upper critical field anisotropy gamma = Hc2//ab/ Hc2//c was found to be temperature dependent (decreasing from 6 at 15 K to 2.8 at 35 K). The effective anisotropy gamma_eff, as calculated from reversible torque data near Tc, is field dependent (increasing roughly linearly from 2 in zero field to 3.7 in 10 kOe). The temperature and field dependence of the anisotropy can be related to the double gap structure of MgB2 with a large two-dimensional gap and small three-dimensional gap, the latter being rapidly suppressed in a magnetic field. Torque magnetometry investigations show a pronounced peak effect, indicating an order-disorder transition of vortex matter. Decoration experiments and STS visualise a hexagonal vortex lattice. STS spectra evidence two gaps (3 meV/6 meV) with direction dependent weight. Magneto-optic investigations with H//c show a clear signature of the smaller of the two gaps, disappearing in fields higher than Hc2//c., Comment: 17 pages pdf only, 15 figures integrated (higher resolution photographs available on request); submitted to Supercond. Sci. Technol. (Proceedings of Boromag conference)

In a recent paper [Phys. Rev. B 66, 012501 (2002)], torque data measured on a MgB2 single crystal in fields from 10 to 60 kOe at 10 K were presented. The authors obtained the anisotropy gamma by fitting a theoretical expression to the data and concluded that the anisotropy is field independent gamma \approx 4.3. They also reported the observation of "intrinsic pinning", which they take as experimental evidence for the occurence of superconductivity in the boron layers. In this comment, we discuss the range of validity of the theoretical expression used by the authors and show that the conclusion of a field independent anisotropy does not hold. Furthermore, we present torque data measured on two crystals of MgB2, establishing the extrinsic nature of the peak in the irreversible torque observed in some crystals., Comment: 3 pages, 2 figures, submitted to Phys. Rev. B Comment on PRB 66, 012501 (2002) (cond-mat/0205010)

We present magneto-optical reflectivity results in the basal-plane of the hexagonal $MgB_2$. The data were collected on a mosaic of $MgB_2$ single crystals with $T_{c}=38 ~K$ from the ultraviolet down to the far infrared as a function of temperature and magnetic field oriented along the c-axis. In the far infrared there is a clear signature of the superconducting gap with a gap-ratio $2\Delta/k_{B}T_{c}\sim 1.2$, well below the weak-coupling value. The gap is suppressed in an external magnetic field, which is a function of temperature. We extract the upper critical field $H_{c2}$ along the c-axis. The temperature dependence of $H_{c2}$ is compatible with the Helfand-Werthamer behaviour., Comment: 6 pages (3 text-pages, 3 figures), submitted to PRL

Measurements of single crystalline MgB2 with torque magnetometry in fields up to 90 kOe reveal a sharp peak in the irreversible torque at about 0.85 Hc2. In the region between peak onset and maximum, pronounced history effects occur. Angle and temperature dependence of the characteristic peak fields track those of Hc2. The features observed suggest that the peak marks a disorder-induced phase transition of vortex matter between a quasi-ordered Bragg glass and a highly-disordered glass., Comment: 4 pages, 4 figures; minor changes, Phys. Rev. B in print

The anisotropy gamma of the superconducting state of high quality single-crystals of MgB2 was determined, using torque magnetometry with two different methods. The anisotropy of the upper critical field was found to be temperature dependent, decreasing from gamma = 6 at 15 K to 2.8 at 35 K. Reversible torque data near Tc reveal a field dependent anisotropy, increasing nearly linearly from gamma = 2 in zero field to 3.7 in 10 kOe. The unusual temperature dependence is a true bulk property and can be explained by non-local effects of anisotropic pairing and/or the wave vector dependence of the effective mass tensor., Comment: RevTex4, 5 pages, 5 figures, some revisions, changed Fig. 5; accepted for publication in PRL

A series of YBa_{2-x}Sr_xCu_4O_8 single crystals was measured to study the influence of site disorder on the transition line Hss(T) between quasi-ordered vortex lattice and highly disordered vortex glass, as well as on the maximum critical current density within the glass phase, jcmax. When 32% of Ba is replaced by Sr, jcmax is an order of magnitude higher than in the unsubstituted compound. In contrast, the transition field Hss first drops by a factor of about five with a substitution of just 10% of Sr for Ba, and then remains approximately constant for higher Sr contents. Our results indicate that in very clean systems the order-disorder transition is affected very strongly by any crystallographic disorder, while above a certain threshold it is relatively robust with respect to additional disorder. In all substituted crystals Hss monotonically decreases with an increase of temperature., Comment: Text revised, some figures replaced, 11 pages, 10 figures, to appear in PRB

The investigation of Zn substitution in MgB2 polycrystalline samples shows that about 0.1 Zn can be substituted in the structure of Mg deficient samples while it can not be substituted in stoichiometric MgB2. As a result of the isovalent Zn substitution into the Mg position of Mg deficient samples the a and c lattice constants increase by about 0.17% and 0.2% respectively. Susceptibility measurements show a slight lowering of Tc by about 0.5 K for 0.05 Zn, which decreases to 0.2 K for 0.1 Zn substitution. Investigation of the pressure derivative of Tc shows dp/dTc = -0.15 K/kbar independent of Zn content. Substitution of Cu leads to multiphase samples without any changes of lattice constants, which indicates that Cu does not enter the structure of MgB2. The Cu substitution broadens the superconducting transition considerably, while the onset remains unchanged., Comment: 13 pages, 5 figures

Oxygen-isotope effect has been investigated in a recently discovered superconductor Sr_{0.4}K_{0.6}BiO_{3}. This compound has a distorted perovskite structure and becomes superconducting at about 12 K. Upon replacing ^{16}O with ^{18}O by 60-80%, the T_c of the sample is shifted down by 0.32-0.50 K, corresponding to an isotope exponent of alpha_{O} = 0.40(5). This isotope exponent is very close to that for a similar bismuthate superconductor Ba_{1-x}K_{x}BiO_{3} with T_c = 30 K. The very distinctive doping and T_c dependencies of alpha_{O} observed in bismuthates and cuprates suggest that bismuthates should belong to conventional phonon-mediated superconductors while cuprates might be unconventional supercondutors., Comment: 9 pages, 5 figures