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Register a new userSingle crystal growth of the pyrochlores $R_2$Ti$_2$O$_7$ ($R$ = rare earth) by the optical floating-zone method
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We report a systematic study on the crystal growth of the rare-earth titanates $R_2$Ti$_2$O$_7$ ($R$ = Gd, Tb, Dy, Ho, Y, Er, Yb and Lu) and Y-doped Tb$_{2-x}$Y$_x$Ti$_2$O$_7$ ($x$ = 0.2 and 1) using an optical floating-zone method. High-quality single crystals were successfully obtained and the growth conditions were carefully optimized. The oxygen pressure was found to be the most important parameter and the appropriate ones are 0.1--0.4 MPa, depending on the radius of rare-earth ions. The growth rate is another parameter and was found to be 2.5--4 mm/h for different rare-earth ions. X-ray diffraction data demonstrated the good crystallinity of these crystals. The basic physical properties of these crystals were characterized by the magnetic susceptibility and specific heat measurements.
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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 crystals. The magnetic susceptibility, isothermal magnetization and heat capacity data of optimally grown crystals are presented.
The results of studies of Y$_{2}$Ti$_2$O$_7$ single crystals doped with Er$^{3+}$ and Yb$^{3+}$ ions by means of electron paramagnetic resonance (EPR) and dc-magnetometry are reported. EPR signals of the trigonal centers with the characteristic hyperfine structure of Er$^{3+}$ or Yb$^{3+}$ ions were observed. Field dependences of magnetization of single crystals for magnetic fields directed along the crystallographic axes and temperature dependences of magnetic susceptibilities were measured. Spin Hamiltonian parameters ($g$-factors and parameters of the hyperfine interaction) for Er$^{3+}$ and Yb$^{3+}$ ions were obtained from analysis of experimental data. The registered EPR spectra and magnetization curves were successfully reproduced by simulations in framework of the crystal-field approach, in particular, with an account for hybridization of ground 4f$^{13}$ configuration of Yb$^{3+}$ ions with the charge transfer states.
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 the synthesis of polycrystalline and single crystal samples are due to the similar thermal stability ranges of different rare-earth silicate compounds in the temperature-composition phase diagrams of the $R$-Si-O systems. The addition of a small amount of SiO$_{2}$ excess allowed the amount of impurity phases present in the powder samples to be minimised. The phase composition analysis of the powder X-ray diffraction data collected on the as-grown boules revealed that they were of single phase, except in the case of thulium disilicate, which comprised of two phases. All growths resulted in multi-grain boules, from which sizable single crystals could be isolated. The optimum conditions used for the synthesis and crystal growth of polycrystalline and single crystal $R_{2}$Si$_{2}$O$_{7}$ materials are reported. Specific heat measurements of erbium and thulium disilicate compounds confirm an antiferromagnetic phase transition below $T_{mathrm{N}}=$ 1.8 K for D-type Er$_{2}$Si$_{2}$O$_{7}$ and a Schottky anomaly centered around 3.5 K in C-type Tm$_{2}$Si$_{2}$O$_{7}$, suggesting the onset of short-range magnetic correlations. Magnetic susceptibility data of E-type Ho$_{2}$Si$_{2}$O$_{7}$ reveals an antiferromagnetic ordering of the Ho spins below $T_mathrm{{N}}=$ 2.3 K.
The very nature of the ground state of the pyrochlore compound Yb$_2$Ti$_2$O$_7$ is much debated, as experimental results demonstrate evidence for both a disordered or a long-range ordered ground state. Indeed, the delicate balance of exchange interactions and anisotropy is believed to lead to competing states, such as a Quantum Spin Liquid state or a ferromagnetic state which may originate from an Anderson-Higgs transition. We present a detailed magnetization study demonstrating a first order ferromagnetic transition at 245 mK and 150 mK in a powder and a single crystal sample respectively. Its first-order character is preserved up to applied fields of $sim$ 200 Oe. The transition stabilizes a ferromagnetic component and involves slow dynamics in the magnetization. Residual fluctuations are also evidenced, the presence of which might explain some of the discrepancies between previously published data for Yb$_2$Ti$_2$O$_7$.
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$^{4+}$.
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