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Register a new userThe pyrochlore Ho2Ti2O7: Synthesis, crystal growth and stoichiometry
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We have investigated the effect of synthesis and growth conditions on the magnetic, structural, and compositional properties of pyrochlore oxide holmium titanate and demonstrate a method for growing high quality stoichiometric single crystals. A series of polycrystalline samples with various contents of Ti (-0.08 leqslant x leqslant 0.08, and nominal compositions of Ho2Ti2+xO7) were synthesized at different temperatures, and characterized using powder X-ray diffraction. The results show that synthesizing powders at a higher temperature of 1500 {deg}C yield single phase compounds. Ti deficient powders showed an increase of lattice constant due to stuffing (Ho into Ti positions), while Ti rich powders showed a decrease in lattice constant due to anti-stuffing (Ti into Ho positions). A post annealing in O2 was found to be necessary to accomplish the anti-stuffing process. Use of the conventional floating zone (FZ) technique introduced Ti deficiency, stuffing, and oxygen vacancies in the grown crystal. Growth of high structural quality and stoichiometric single crystals of Ho2Ti2O7 by the traveling solvent floating zone (TSFZ) is reported. AC susceptibility measurements revealed that the stoichiometric crystal shows a higher ice freezing temperature, indicating that crystal quality and stoichiometry play a key role on low temperature spin ice properties of this compound.
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Pyrochlore $rm Pr^{3+}_{2+x}Zr^{4+}_{2-x}O_{7-x/2}$ samples in the form of both powders $(-0.02 le x le 0.02)$ and bulk single crystals have been studied to elucidate the dependence of their magnetic, compositional and structural properties on synthesis and growth conditions. All samples were characterized using X-ray diffraction, specific heat, and DC magnetization measurements. The crystals were also studied using the X-ray Laue technique and scanning electron microscopy. Increasing the Pr content for the $rm Pr_{2+x}Zr_{2-x}O_{7-x/2}$ powders enlarged the lattice parameter, and resulted in systematic changes in magnetic susceptibility and specific heat. Stoichiometric and high quality single crystals of $rm Pr_2Zr_2O_7$ were grown using the optical floating zone technique under a high purity static argon atmosphere, to avoid inclusions of Pr$^{4+}$ and limit Pr vaporization. Increasing the growth speed was found to significantly reduce Pr vaporization for better control of stoichiometry. Scanning electron microscopy provided direct evidence of spinodal decomposition during growth that is controllable via rotation rate. An intermediate rotation rate of 3-6 rpm was found to produce the best microstructure. The magnetic susceptibility of crystals grown at rates from 1-20 mm/hr revealed changes that were consistent with Pr vaporization. Further, we report indications of local off-centering of Pr$^{3+}$ ions from the ideal pyrochlore sites, similar to what is known for the trivalent cation in $rm Bi_2Ti_2O_7$ and $rm La_2Zr_2O_7$. The effect varies with Pr content and radically modulates the low temperature specific heat. Overall, the results clearly demonstrate important correlations between the growth conditions and physical properties of $rm Pr_2Zr_2O_7$ crystals.
Terbium titanate (Tb$_2$Ti$_2$O$_7$) is a spin-ice material with remarkable magneto-optical properties. It has a high Verdet constant and is a promising substrate crystal for the epitaxy of quantum materials with the pyrochlore structure. Large single crystals with adequate quality of Tb$_2$Ti$_2$O$_7$ or any pyrochlore are not available so far. Here we report the growth of high-quality bulk crystals using the Czochralski method to pull crystals from the melt. Prior work using the automated Czochralski method has suffered from growth instabilities like diameter fluctuation, foot formation and subsequent spiraling shortly after the seeding stage. In this study, the volumes of the crystals were strongly increased to several cubic centimeters by means of manual growth control, leading to crystal diameters up to 40 mm and crystal lengths up to 10 mm. Rocking curve measurements revealed full width at half maximum values between 28 and 40 for 222 reflections. The specific heat capacity c$_p$ was measured between room temperature and 1573 K by dynamic differential scanning calorimetry and shows the typical slow parabolic rise. In contrast, the thermal conductivity kappa(T) shows a minimum near 700 K and increases at higher temperature T. Optical spectroscopy was performed at room temperature from the ultraviolet to the near infrared region, and additionally in the near infrared region up to 1623 K. The optical transmission properties and the crystal color are interpreted to be influenced by partial oxidation of Tb$^{3+}$ to Tb$^{4+}$.
We have successfully grown cm3-size single crystals of the metallic-ferromagnet Sm2Mo2O7 by the floating-zone method using an infrared-red image furnace. The growth difficulties and the remedies found using a 2-mirror image furnace are discussed. Magnetization studies along the three crystalline axes of the compound are presented and discussed based on our recent proposal of an ordered spin-ice ground state for this compound
Inelastic neutron scattering was employed to study the crystal-field interaction in the strontium-doped rare-earth compounds R(x)Sr(1-x)CoO(3-z) (R=Pr, Nd, Ho, and Er). Particular emphasis is laid on the effect of oxygen deficiencies which naturally occur in the synthesis of these compounds. The observed energy spectra are found to be the result of a superposition of crystal fields with different nearest-neighbor oxygen coordination at the R sites. The experimental data are interpreted in terms of crystal-field parameters which behave in a consistent manner through the rare-earth series, thereby allowing a reliable extrapolation for rare-earth ions not considered in the present work.
Inelastic neutron scattering measurement is performed on a breathing pyrochlore antiferromagnet Ba3Yb2Zn5O11. The observed dispersionless excitations are explained by a crystalline electric field (CEF) Hamiltonian of Kramers ion Yb3+ of which the local symmetry exhibits C3v point group symmetry. The magnetic susceptibility previously reported is consistently reproduced by the energy scheme of the CEF excitations. The obtained wave functions of the ground state Kramers doublet exhibit the planer-type anisotropy. The result demonstrates that Ba3Yb2Zn5O11 is an experimental realization of breathing pyrochlore antiferromagnet with a pseudospin S = 1/2 having easy-plane anisotropy.
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