Zone Melting Research Articles

Insight into faceted-nonfaceted transition of directionally solidified eutectic ceramic composites by laser floating zone melting and infrared imaging

Faceted-nonfaceted transition was found during directional solidification of an Al2O3/Y3Al5O12(YAG)/ZrO2 eutectic ceramic composite at the pulling rate over 260 μm/s by laser floating zone melting. This transition, for the first time, optimized the colony structure of faceted eutectic composite materials, resulting in a refined and homogeneous microstructure consisting of both rod and lamella. Infrared imaging was employed to uncover temperature field evolution of the melt during the transition relying on an interesting measurement calibration strategy. In addition to an in-depth discussion about this evolution, we revealed that the transition was triggered by a critical undercooling at the solid-liquid interface. A 3D model of this novel eutectic structure was established, by which the mechanism of structural optimization achieved by the transition was discussed. We supposed that the growth orientation with the smallest index could firstly occur faceted-nonfaceted transition under a certain undercooling degree, and subsequently predominated the growth of faceted eutectic composite, which contributed to the optimization of faceted eutectic colony structure.

Metallurgical Properties of Vacuum Extrusion Iron‐Rich Dust Briquette and Its Effects on Blast Furnace Soft Melting Zone

The vacuum extrusion iron‐rich dust briquette (VEIDB) in this study is prepared by vacuum extrusion of iron ore fines and blast furnace dust. In this article, the metallurgical properties such as compressive strength, tumbler strength, low temperature reduction disintegration performance, reducibility, and softening melting properties of VEIDB are studied. The effect of VEIDB on the soft melting zone of blast furnace is also studied. Results show that the compressive strength of VEIDB is 5.684 kN/VEIDB, the tumbler strength is 89.87%, RDI−0.5 = 2.82%, and the metallization degree after reduction is 96.9%. However, its softening and melting properties is bad. The study on the influence of VEIDB on softening and melting properties of iron‐containing burden shows that, adding VEIDB in blast furnace burden would make the soft melting zone of blast furnace move up and expand; with the increase of the VEIDB amount, the permeability decreases first and then increases. The addition of VEIDB in blast furnace burden should be controlled within 10%.

Advances in high-pressure laser floating zone growth: The Laser Optical Kristallmacher II (LOKII).

The optical floating zone crystal growth technique is a well-established method for obtaining large, high-purity single crystals. While the floating zone method has been constantly evolving for over six decades, the development of high-pressure (up to 1000bar) growth systems has only recently been realized via the combination of laser-based heating sources with an all-metal chamber. While our inaugural high-pressure laser floating zone furnace design demonstrated the successful growth of new volatile and metastable phases, the furnace design faces several limitations with imaging quality, heating profile control, and chamber cooling power. Here, we present a second-generation design of the high-pressure laser floating zone furnace, "Laser Optical Kristallmacher II" (LOKII), and demonstrate that this redesign facilitates new advances in crystal growth by highlighting several exemplar materials: α-Fe2O3, β-Ga2O3, and La2CuO4+δ. Notably, for La2CuO4+δ, we demonstrate the feasibility and long-term stability of traveling solvent floating zone growth under a record pressure of 700bar.

Characterization of scintillation properties in Ca(Nb,Ta)2O6 single crystals

CaNb2-xTaxO6 (x = 0, 0.2, 0.5 and 1) single crystals were fabricated by the floating zone method, and their photoluminescence (PL) and scintillation properties were evaluated. Under excitation at 280 nm, CaNb2-xTaxO6 single crystal showed a broad emission band at 400–600 nm. From the decay time constant, the observed emission was attributed to the charge transfer (CT) from the Nb5+ to the O2−. Under X-ray irradiation, an emission peak was observed at 470 nm, and the scintillation decay time profile suggested that the origin of the emission was also CT from the Nb5+ to the O2−. CaNb2O6 showed the highest light yield of 15,000 ph/MeV and the lowest afterglow level of 6.03 ppm among the synthesized samples.

Effect of laser wavelength on the thermoelectric properties of Bi1.6Pb0.4Sr2Co2O8 textured ceramics processed by LFZ

Bi1.6Pb0.4Sr2Co2O8 samples have been textured by the Laser Floating Zone (LFZ) process using Nd:YAG, and CO2 laser radiation. Using different wavelengths resulted in significant structural and microstructural modifications. Powder XRD patterns showed that the thermoelectric phase is the major one in both cases. Microstructural studies revealed that all samples presented the same phases but with much lower content of secondary ones in those processed with the CO2 laser. Electrical resistivity showed different behavior for the two types of samples, being in general, lower for the CO2 grown rods. Seebeck coefficient is lower for the CO2 grown samples up to 300 °C, and higher in the high-temperature range, reaching 240 μV/K at 650 °C, which is one of the highest values obtained so far in these compounds. Moreover, thermal conductivity at 600 °C for these samples (0.93 W/K m) is among the lowest reported in the literature. As a consequence, ZT values at 600 °C reached 0.42 in CO2 textured materials, about two times higher than the obtained in Nd:YAG ones. This value is among the highest reported so far in the literature, and is comparable to the performance attained for the same composition containing nanoparticles addition. All these properties, combined with the fact that the processed materials can be directly integrated into thermoelectric modules, render them highly attractive for industrial production.

Structure and magnetic properties of a La0.75Sr0.25Cr0.90O[formula omitted] single crystal

We have successfully grown large and good-quality single crystals of the La0.75Sr0.25Cr0.90O3−δ compound using the floating-zone method with laser diodes. We investigated the crystal quality, crystallography, chemical composition, magnetic properties and the oxidation state of Cr in the grown single crystals by employing a combination of techniques, including X-ray Laue and powder diffraction, scanning electron microscopy, magnetization measurements, X-ray photoelectron spectroscopy and light absorption. The La0.75Sr0.25Cr0.90O3−δ single crystal exhibits a single-phase composition, crystallizing in a trigonal structure with the space group R3̄c at room temperature. The chemical composition was determined as La0.75Sr0.25Cr0.90O3−δ, indicating a significant chromium deficiency. Upon warming, we observed five distinctive characteristic temperatures, namely T1=21.50(1) K, T2=34.98(1) K, T3=117.94(1) K, T4=155.01(1) K, and TN=271.80(1) K, revealing five distinct magnetic anomalies. Our magnetization study allows us to explore the nature of these anomalies. Remarkably, the oxidation state of chromium in the single-crystal La0.75Sr0.25Cr0.90O3−δ, characterized by a band gap of 1.630(8) eV, is exclusively attributed to Cr3＋ ions, making a departure from the findings of previous studies on polycrystalline materials.

Up- and down-conversion photoluminescence properties of Ho2O3 doped YbAG single crystals prepared by optical floating zone method

Single crystals of garnets with composition Yb2.96-xYxHo0.04Al5O12 (x = 0, 2.92, 2.96) were grown by optical floating zone method, and shown by XRD measurements to be in the cubic phase. EDS spectra show that Ho3+ and Yb3+ were homogenously distributed in the structure. As shown by the transmission and absorption spectra, the Yb2.96-xYxHo0.04Al5O12 crystals are highly transparent and can function as excellent optical crystals. Compared to the Y2.96Ho0.04Al5O12 crystal, the Yb2.96Ho0.04Al5O12 crystal has an additional strong broad absorption in the 836–1070 nm range, which increases its absorption of 980 nm photons. The optical band gaps of the Yb2.96-xYxHo0.04Al5O12 crystals decrease with increasing Yb2O3 concentration. Furthermore, differences with Yb2O3 concentrations in the Yb2.96-xYxHo0.04Al5O12 crystals were observed for the first time in the up- and down-conversion photoluminescence. Under excitation with a 980 nm laser, the up-conversion PL spectra of the Yb2.96-xYxHo0.04Al5O12 crystals show several emission peaks at 548 nm, 665 nm and 775 nm, and their intensities increase with Yb2O3 concentrations. In the Yb2.96Ho0.04Al5O12 crystal, Yb3+ not only is a component of the garnet structure, but it also acts as a sensitizer. In regards of down-conversion, under excitation at 454 nm, the down-conversion PL spectra of the Yb2.96-xYxHo0.04Al5O12 crystals show strong emission peaks at 550 nm, and their intensities decrease with increasing Yb2O3 concentrations, which is considered to be the consequence of increasing matrix density.

Spin reorientation, spin switching, and magnetic compensation in Er1−xSmxFeO3 single crystals

We investigated spin reorientation, magnetic compensation and spin switching transitions in a series of high-quality single crystals of Er1−xSmxFeO3 (x = 0, 0.2, 0.4, 0.6, 0.8) prepared using the optical floating zone method. Structural and other preliminary characterizations confirmed the quality and phase purity of the crystals. Rietveld refinement of powder XRD data indicates that lattice parameters a and c increase linearly with increasing Sm concentration, whereas b remained constant. Field-cooled cooling (FCC) measurements revealed a temperature-induced spin reorientation transition (SRT) from Γ4 (Gx, Ay, Fz) to Γ2 (Fx, Cy, Gz) for all the samples. SRT temperature increased with Sm concentration and spread widely above and below room temperature. Moreover, magnetic compensation is common to all the compositions but decreases as Sm doping increases. We also observe type-I spin switching in samples with x = 0, 0.2, and 0.4 at an applied field of 60 Oe under FCC protocol, with a reduction in spin switching temperature as Sm content increased. For Sm-rich samples (x = 0.6, 0.8), spin switching was absent at 60 Oe.

Process Optimization in Laser Welding of IN792 DS Superalloy

Ni-base superalloys are employed to produce parts of aeronautic engines, space vehicles and power plants. During the production process or lifetime of components, cracks may occur which affect their performance. Reliable repairs can be carried out through high-energy density welding techniques. This work investigated laser welding of the directionally solidified IN792 DS superalloy. The characteristics of the original material and their evolution in the base metal, heat-affected zone and melt zone after laser welding in different conditions and post-welding heat treatment were investigated through micro-hardness tests, light and scanning electron microscopy observations. The study allowed to optimize the process parameters and post-welding heat treatment, obtaining joints without macro-defects, such as cracks and pores, and with properties and microstructures of the melt zone like those of base metal.

Effect of High-Frequency Electric Pulse on the Solidification Microstructure and Properties of Hypoeutectic Al-Si Alloy.

The effects of different pulse frequencies on the microstructure grain size and solid solubility of Al-9Si alloy were systematically investigated using OM, SEM, and EDS. The impact on the mechanical properties of the alloy was analyzed using a micro-Vickers hardness tester and multifunctional friction tester. During solidification, the Al-9Si alloy is exposed to high-frequency electric current pulses with a current density of 300 A/cm2 and frequencies of 0 Hz, 500 Hz, 1000 Hz, and 2000 Hz. The experimental results show that the Lorentz force also increases as the high-frequency pulse frequency increases. Intense electromagnetic stirring leads to grain refinement. However, as the pulse frequency continues to grow, the combined effect of Joule heating and Lorentz force results in an enlargement of the melt zone and an increase in grain size. At a pulse frequency of 1000 Hz, the eutectic structure size of the Al-9Si alloy is optimal, with the average size being reduced to 13.87 μm and a dense distribution, effectively eliminating primary Si. The EDS results revealed that the high-frequency pulse led to a more uniform distribution of Si elements within the matrix, and the solid solubility of Si in the α-Al matrix increased to a maximum value of 1.99%, representing a 39.2% increase. At a pulse frequency of 1000 Hz, the sample demonstrates the most favorable mechanical properties, with the friction coefficient reaching a minimum value of 0.302, representing a 37.7% decrease in the average friction coefficient. The results demonstrate that high-frequency pulsing is an effective method for enhancing the mechanical properties of Al-9Si alloy.

Time–temperature correlations of amorphous thermoplastics at large strains based on molecular dynamics simulations

In this paper, we investigate the time–temperature correlation of amorphous thermoplastics at large strains based on coarse-grained molecular dynamics simulations. This correlation behavior is characterized by the strain hardening modulus in uniaxial tension simulations at different strain rates across the glass transition region. The temperature regime is divided into a melt zone, a glassy zone, and a transition zone between them, according to the storage modulus calculated from dynamic mechanical analysis (DMA) at small strains. In the melt zone, the existence of time–temperature superposition (TTS) at large strains is verified by constructing a master curve of the hardening modulus. The obtained shift factors are then compared to those from DMA at small strains, showing that the TTS behavior is transferable between small and large strains. In the glassy zone, the effects of time and temperature are not superposable at large strains but still can be correlated. To demonstrate this correlation behavior, we introduce a level set of the hardening modulus with a variable pair of strain rate and temperature. Pairs lying in the same level result in coincident stress–strain curves at large strains. The transferability of the correlation behavior between large and small strains is validated by comparing these stress–strain curves at small strains in the pre-yield region. In the transition zone, the correlation behavior is studied with both aforementioned methods, showing that TTS is applicable to large strains but not transferable to small strains. Finally, we propose a phenomenological constitutive model for uniaxial tension to demonstrate the time–temperature correlation at large strains, considering different constant strain rates and temperatures.

Investigation and optimisation of a lithium-drift silicon detector using Si–Li structure and bidirectional diffusion and drift techniques

Abstract The research relevance is predefined by the continuous development and improvement of radiation analysis methods and the need for more efficient and accurate detectors for various applications. This research may improve the sensitivity and resolution of Si(Li) detectors, which is important for scientific and industrial research as well as radiation safety monitoring. The research aims to analyse and improve the performance of a Si(Li) lithium-drift silicon detector. The methods used include an analytical method, classification method, functional method, statistical method, synthesis method and others. The results of the two-sided observation of lithium diffusion in silicon monocrystals provided valuable information about the characteristics of the process and its dependence on the method of silicon production. A large-diameter detector detection mode was found to be important for optimising the production of such detectors. The diffusion process in monocrystalline silicon produced by the shadowless zone melting method is relatively fast. This means that lithium ions penetrate the material rapidly and spread evenly throughout its volume. This fast diffusion process can be useful for detectors that need to respond quickly to incoming signals. It was found that in monocrystalline silicon produced by the Czochralski method, there is a delayed penetration of lithium ions.

Magnetic Characterization of Zone-Refined Rare-Earth Orthoferrite Crystals Grown by the Optical Floating Zone Method

Magnetic Characterization of Zone-Refined Rare-Earth Orthoferrite Crystals Grown by the Optical Floating Zone Method

Experimental Analysis of High Purity Tellurium Prepared by Zone Refining

Experimental Analysis of High Purity Tellurium Prepared by Zone Refining

Simulation of thermal processes in a half-space under heating by a moving source with a uniformly distributed heat flow

Using the method of applying instantaneous point sources, a solution was obtained to the problem of heat conduction during surface heating of a body in the form of a half-space by a uniformly distributed highly concentrated heat flux moving at a constant speed along a rectilinear trajectory with a different shape of the heating spot at constant thermophysical characteristics of the material. The effect of temperature loading modes and the shape of the heating spot on thermal processes in the heat-affected zone is studied. The surfaces and lines of the temperature level are constructed for different moments of time and speed loading modes in different planes of the heating zone. Time dependences of temperatures, heating and cooling rates for body points are given. The shortcomings of the methods used for linear thermal conductivity, the lack of direct consideration in the design scheme of the surface melt zone of the material do not allow one to reliably assess the effect of heat treatment modes on changes in material properties, focusing only on the level of the maximum design temperature. In this regard, the structure formation of metal in the zone of thermal action is proposed to be associated with a thermal impulse, i.e. the total thermal energy perceived by the material at a given point of the body, as well as with the effective structurization impulse introduced into consideration, which characterizes the energy spent on the process of structural transformations of the material, and the structurization time at a point and some volume of the body. The dependencies of these values on the speed of movement and the shape of the heating spot are presented. The considered approaches can be applied to various metals and alloys. The research results can be used to develop more effective methods for determining the optimal modes of surface hardening of metal products with a high-energy source.

High-performance Bi0.4Sb1.6Te3 alloy prepared by a low-cost method for wearable real-time power supply and local cooling

Manufacturing low-cost, high-performance thermoelectric (TE) modules is essential for power generation and cooling. However, traditional fabrication methods (zone melting and hot pressing) are time-consuming and expensive, and the fabricated Bi2Te3-based materials have unsatisfied performance. Herein, Bi0.4Sb1.6Te3 alloys with high TE properties were prepared using cold pressing and thermal annealing processes. This preparation process is simple, time saving, and suitable for large-scale promotion. The annealing process induces the formation of pores within the grain interface, which effectively scatters low-energy charge carriers and enhance the phonon scattering. Although the electrical properties is reduced, the improved Seebeck coefficient compensates for the deteriorated electrical properties. Meanwhile, the thermal conductivity is significantly reduced. Eventually, a peak ZT of ∼1.27 is achieved at 333 K. The TE modules assembled with our Bi0.4Sb1.6Te3 alloy exhibit high output and cooling performance, with an output power density of 12.62 mW/cm2 with a temperature difference of 30 K. Furthermore, the TE module can be used for the active cooling of human skin and achieve a cooling effect of ∼8.0 °C. These results indicate that our samples are suitable for the preparation of commercially applicable TE modules and as power sources for next-generation wearable electronic devices.

Impact of Convection and Rotation on Advanced Thermal Energy Storage Using Nanoencapsulated Phase Change Materials in Wavy Enclosures

Free convection heat transfer in hybrid nanofluids in a differentially heated wavy enclosure is studied. The wavy enclosure moves at a constant counterclockwise rotational speed along its longitudinal axis. The enclosure is filled with a hybrid nanofluids consisting of water (H2O) and nanoencapsulated phase change materials (NEPCMs). These NEPCMs consist of a polyurethane coating and a core of N‐nonadecane, which undergoes a phase transition and has the capacity to retain or emit a significant quantity of latent heat. The dimensionless forms of the governing equations have been solved using finite element method. The validity of the present code is demonstrated by comparing its predictions with published results. The governing parameters under consideration are the corrugated number, 0 ≤ N ≤ 3, the volume fraction of hybrid nanoparticles, 0.0 ≤ ϕ ≤ 0.05, the Taylor number, 8 × 102 ≤ TaH2O ≤ 2 × 104. Changing the rotation speed is found to alter the melting and solidification zones in terms of pathways and size zones. The melting zone has a large size at moderate wave number, and its size shrinks and shifts downward as the wave number increases. An increase in the heat transfer rate values up to 38% is obtained when the concentration is adjusted from 1% to 5% for N = 1.

High-quality Indium-doped Gallium Oxide Single Crystal Growth by Floating Zone Method

High-quality Indium-doped Gallium Oxide Single Crystal Growth by Floating Zone Method

Bulk crystal growth and characterization of non-centrosymmetric single crystal CaTa4O11

For the first time, high-quality bulk single crystals of CaTa4O11 were grown by the floating-zone method, and thus the current phase-diagram was revised for the stoichiometry CaO·2Ta2O5, showing a congruent melting behavior.

Особенности фазовых и структурных превращений в композиционных материалах на основе систем несмешивающихся компонентов при воздействии концентрированных потоков энергии

The features of phase and structural transformations in composite materials based on systems of immiscible components Al – Be, Al – Be – Mg, Fe – Cu, Fe – Cu – Pb under the influence of concentrated heat sources — electric arc, electron and laser beams — are considered. It is shown that when materials of the Al – Be, Al – Be – Mg systems are exposed to an electric arc plasma and an electron flow, they are melted and subsequently cooled by grain grinding, formation of a zone of thermal influence and crystallization of the resulting new structures and phases. In zone of thermal influence, the enrichment of the aluminum matrix with Be particles is observed due to the thermal diffusion processes of their movement. When plasma is exposed to an arc discharge, pulsed and continuous laser radiation, as well as the flow of electrons on the composition Fe – Cu, Fe – Cu – Pb, a change in the morphology of the near-surface layer is observed: the irradiated material in the melt zone is exfoliated and in the process of crystallization the stratified phases are fixed in a solid state. The mechanism of stratification formation is associated with the limited solubility of the elements that make up the composition in the liquid and solid states.