Advances in Crystal Growth: Pioneering Materials for Tomorrow's Technologies

A special issue of Crystals (ISSN 2073-4352). This special issue belongs to the section "Crystal Engineering".

Deadline for manuscript submissions: closed (20 September 2024) | Viewed by 8146

Special Issue Editors


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Guest Editor
Crystal Growth Facility, Institute of Physics, École Polytechnique Fédérale de Lausanne, CH-1015 Lausanne, Switzerland
Interests: flux method; floating zone technique; high temperature and high-pressure growth; superconducting and magnetic materials

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Guest Editor
Crystal Growth Facility, Institute of Physics, École Polytechnique Fédérale de Lausanne, CH-1015 Lausanne, Switzerland
Interests: materials discovery; crystal growth; nanostructures synthesis; structure determination; study of crystal growth mechanism

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Guest Editor
Crystal Growth Facility, Institute of Physics, École Polytechnique Fédérale de Lausanne, CH-1015 Lausanne, Switzerland
Interests: X-Ray crystallography

Special Issue Information

Dear Colleagues,

Materials are the cornerstone of technological advancement, driving innovations across various sectors. High-performance energy-related applications, including photovoltaics, fuel cells, batteries and thermoelectrics, as well as information and data storage technologies, heavily rely on the development of novel materials.

However, synthesizing high-quality single crystals for in-depth characterization remains a formidable challenge. Issues arise from incongruent melting behavior, rapid evaporation rates, high melting points, and the absence of precise phase diagrams for complex solute–solvent systems. Trial and error continues to dominate crystal growth techniques.

This Special Issue delves into recent advancements in crystal growth methods for novel compounds and emerging growth technologies. Emphasis is placed on solvent design and selection for flux-based growth of high-quality single crystals, as well as the impact of growth conditions on desired phase formation and quality optimization. Crucial aspects of crystal growth, such as solute–solvent phase diagrams, growth mechanisms, and solvent transport properties, are explored. Experiments combined with a solvent–solution system design promise to expedite crystal growth and enhance crystal quality. Although direct observation of crystal growth remains challenging, indirect monitoring of precipitation and growth allows for control of growth parameters.

The crystal growth process inherently fosters material exploration and discovery. Experimental phase diagram studies can unveil previously unknown phases and structures, while doping and modification of existing structures efficiently yield new materials.

This Special Issue of Crystals brings together cutting-edge research that not only contributes to the growth of novel compounds but also enhances our grasp of the fundamental science behind crystal growth. It stands as a testament to the relentless pursuit of innovation in the world of materials science.

Dr. Yong Liu
Dr. Arnaud Magrez
Dr. David Wen Hua Bi
Guest Editors

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Keywords

  • crystal growth of novel materials
  • design of solvent–solution systems
  • flux growth
  • floating zone growth
  • chemical vapour transport

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Published Papers (7 papers)

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Research

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13 pages, 7188 KiB  
Article
Structural, Morphological, and Optical Properties of Nano- and Micro-Structures of ZnO Obtained by the Vapor–Solid Method at Atmospheric Pressure and Photocatalytic Activity
by Carlos Bueno, Adan Luna, Gregorio Flores, Héctor Juárez, Mauricio Pacio, René Pérez, Javier Flores-Méndez, David Maestre and Raúl Cortés-Maldonado
Crystals 2024, 14(11), 941; https://doi.org/10.3390/cryst14110941 - 30 Oct 2024
Viewed by 221
Abstract
Micro- and nano-structures of ZnO were synthesized by the vapor–solid method at 600, 700, and 800 °C in atmospheres of Ar and air, at atmospheric pressure. The structural characterization XRD shows that the nano-structures synthesized in air atmosphere at 600 °C, while diffraction [...] Read more.
Micro- and nano-structures of ZnO were synthesized by the vapor–solid method at 600, 700, and 800 °C in atmospheres of Ar and air, at atmospheric pressure. The structural characterization XRD shows that the nano-structures synthesized in air atmosphere at 600 °C, while diffraction peaks were found due to Zn because the presence of metallic Zn remains on the surface of the pellet. SEM images show that the morphologies range from nano-wires to micro-tubes. When cathodoluminescence is measured in micro-tubes, there is a shift of the near-band edge of the ZnO toward red; this is due to structural defects in the ZnO network. This result is corroborated with panchromatic CL measurements, which exhibit a difference in brightness between the micro-tubes. Furthermore, EDS measurements show an atomic quantity ratio of Zn:O that differs from the stoichiometric composition in the micro-tubes. The photocatalytic activity of three types of structures—nano-wires, micro-tubes, and micro-rods under UV irradiation using methylene blue as a model pollutant—were evaluated. The best response was obtained for nanowires, not only because they have a larger surface area but also because of the present defects. Full article
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12 pages, 3792 KiB  
Article
The Influence of In3+ on the Crystal Growth and Visible Band Photorefraction of Uranium-Doped Lithium Niobate Single Crystals
by Tian Tian, Wenjie Xu, Chenkai Fang, Yuheng Chen, Hongde Liu, Yaoqing Chu, Hui Shen and Jiayue Xu
Crystals 2024, 14(4), 380; https://doi.org/10.3390/cryst14040380 - 18 Apr 2024
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Abstract
A series of lithium niobate crystals co-doped with uranium and indium was successfully grown by the modified vertical Bridgman method for the first time. With increasing In3+ ion doping concentration, the segregation coefficient of uranium and indium progressively deviated from 1. The [...] Read more.
A series of lithium niobate crystals co-doped with uranium and indium was successfully grown by the modified vertical Bridgman method for the first time. With increasing In3+ ion doping concentration, the segregation coefficient of uranium and indium progressively deviated from 1. The structural refinement indicated that uranium ions with high valence preferred to occupy the Nb sites in LN: In, U crystals. LN: In2.0, U0.6 achieved multi-wavelength holographic writing with diffraction efficiency comparable to commercial crystals LN:Fe0.3, demonstrating a response time that was four times shorter than LN:Fe0.3. XPS analysis was employed to investigate the valence states of In3+ ions in LN: In2.0, U0.6, in which uranium ions presented three valences of +4, +5 and +6. Furthermore, the ‘real threshold concentration’ of In3+ ions in LN: In, U was calculated using the Li-vacancy model, which is consistent with the results obtained from the experimental study of the OH absorption spectrum. Discussions on the photorefractive centers in LN: In, U are also provided. This study not only demonstrates the impact of doping In3+ ions on the growth of LN:U crystals, but also offers new insights into the photorefractive properties of LN in the visible band. Full article
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10 pages, 6141 KiB  
Article
Growth of Spontaneous Nucleation AlN Crystals by Al-Base Alloy Evaporation in Nitrogen Atmosphere
by Xiaochun Tao, Yongkuan Xu, Jianli Chen, Yonggui Yu, Xiaofang Qi, Wencheng Ma and Zhanggui Hu
Crystals 2024, 14(4), 331; https://doi.org/10.3390/cryst14040331 - 30 Mar 2024
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Abstract
Aluminum nitride (AlN) crystals with areas ranging from 1 mm2 to 2 mm2 were successfully grown through spontaneous nucleation at 1700 °C using a modified vapor transport method. In this approach, Cu–Al alloy served as the source of aluminum (Al), and [...] Read more.
Aluminum nitride (AlN) crystals with areas ranging from 1 mm2 to 2 mm2 were successfully grown through spontaneous nucleation at 1700 °C using a modified vapor transport method. In this approach, Cu–Al alloy served as the source of aluminum (Al), and nitrogen (N2) was employed as the nitrogen source. The morphology and crystalline quality of the AlN crystals were characterized by a stereo microscope, Raman spectrometer, photoluminescence (PL) and secondary-ion mass spectrometry (SIMS). Deposited on the graphite lid, the as-grown AlN crystals exhibited both rectangular and hexagonal shapes, identified as m-plane and c-plane AlN, respectively, based on Raman spectroscopy. The full width half maximum (FWHM) values of E2 (high) for the rectangular and hexagonal grains were measured to be 6.00 cm−1 and 6.06 cm−1, respectively, indicating high crystalline quality. However, PL and SIMS analysis indicated the presence of impurities associated with oxygen in the crystals. This paper elucidates the growth mechanism of the modified vapor transport method and highlights the role of the Cu–Al alloy in sustaining reactions at lower temperatures. The addition of copper (Cu) not only facilitates sustainable reactions, but also provides a novel perspective for the growth of AlN single crystals. Full article
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10 pages, 3018 KiB  
Article
On Melt Growth and Microstructure Characterization of Magnesium Bicrystals
by Kevin Bissa, Talal Al-Samman and Dmitri A. Molodov
Crystals 2024, 14(2), 130; https://doi.org/10.3390/cryst14020130 - 27 Jan 2024
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Abstract
Oriented magnesium bicrystals with a 45°101¯0 asymmetrical tilt boundary were produced by directional solidification in a vertical Bridgman furnace. Employing a partition in the cylindrical mold led to unwanted crystallization on the contact surface with the growing interface, disrupting [...] Read more.
Oriented magnesium bicrystals with a 45°101¯0 asymmetrical tilt boundary were produced by directional solidification in a vertical Bridgman furnace. Employing a partition in the cylindrical mold led to unwanted crystallization on the contact surface with the growing interface, disrupting the desired growth conditions for the boundary. A modified setup with seed crystals placed side by side in a conical mold addressed the former issue and enabled the production of high-quality 56 mm × 34 mm bicrystals. Due to the asymmetrical character of the boundary, the adjacent growing crystals witnessed unequal growth rates, with the basal-oriented crystal dominating the growth process. Plane strain compression experiments were carried out on bicrystalline samples extracted from the prepared bicrystal. The panoramic orientation mapping of large areas of several mm2 revealed low-angle boundaries (5° misorientation) associated with the curved segments of the original asymmetrical tilt boundary. It also depicted heterogeneous lattice rotation near the grain boundaries. Full article
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14 pages, 6974 KiB  
Article
Crystal Growth of the R2SiO5 Compounds (R = Dy, Ho, and Er) by the Floating Zone Method Using a Laser-Diode-Heated Furnace
by Vasile Cristian Ciomaga Hatnean, Aurel Pui, Arkadiy Simonov and Monica Ciomaga Hatnean
Crystals 2023, 13(12), 1687; https://doi.org/10.3390/cryst13121687 - 14 Dec 2023
Cited by 2 | Viewed by 1516
Abstract
In recent years, rare earth silicate compounds have attracted the extensive attention of researchers owing to their potential for applications in scintillation crystals in gamma ray or X-ray detectors, as well as in thermal or environmental barrier coatings. Large high quality crystals of [...] Read more.
In recent years, rare earth silicate compounds have attracted the extensive attention of researchers owing to their potential for applications in scintillation crystals in gamma ray or X-ray detectors, as well as in thermal or environmental barrier coatings. Large high quality crystals of three members of the rare earth monosilicates family of compounds, R2SiO5 (with R = Dy, Ho, and Er), have been grown by the floating zone method, using a laser-diode-heated floating zone furnace. Crystal growths attempts were carried out using different parameters in order to determine the optimum conditions for the growth of these materials. The phase purity and the crystalline quality of the crystal boules were analysed using powder and Laue X-ray diffraction. Single crystal X-ray diffraction experiments were carried out to determine the crystal structures of the boules. The optimum conditions used for the crystal growth of R2SiO5 materials are reported. The phase purity and high crystalline quality of the crystals produced makes them ideal for detailed investigations of the intrinsic physical and chemical properties of these materials. Full article
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18 pages, 4236 KiB  
Article
A Coupled Approach to Compute the Dislocation Density Development during Czochralski Growth and Its Application to the Growth of High-Purity Germanium (HPGe)
by Wolfram Miller, Andrejs Sabanskis, Alexander Gybin, Kevin-P. Gradwohl, Arved Wintzer, Kaspars Dadzis, Jānis Virbulis and Radhakrishnan Sumathi
Crystals 2023, 13(10), 1440; https://doi.org/10.3390/cryst13101440 - 28 Sep 2023
Cited by 1 | Viewed by 1196
Abstract
The evolution of the dislocation density during Czochralski growth is computed by the combination of global thermal calculations and local computation of the stress and dislocation density in the crystal. The global simulation was performed using the open-source software Elmer (version 8.4) and [...] Read more.
The evolution of the dislocation density during Czochralski growth is computed by the combination of global thermal calculations and local computation of the stress and dislocation density in the crystal. The global simulation was performed using the open-source software Elmer (version 8.4) and the local simulation with the open-source software MACPLAS (version of 23.1.2023). Interpolation both in space and time was used to transfer the boundary conditions from the global simulations to the local model, which uses a different mesh discretization and a considerably smaller time step. We applied this approach to the Czochralski growth of a high-purity Ge crystal. The heater power change predicted by the global model as well as the final dislocation density distribution in the crystal simulated by the local model are correlated to the experimental results. Full article
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Review

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21 pages, 11142 KiB  
Review
Recent Progress of Floating-Zone Techniques for Bulk Single-Crystal Growth
by Naoki Kikugawa
Crystals 2024, 14(6), 552; https://doi.org/10.3390/cryst14060552 - 14 Jun 2024
Viewed by 1536
Abstract
This review describes the recent progress of floating-zone techniques for bulk single-crystal growth. The most crucial point of the crucible-free technique is to keep the molten zone stable. It has been investigated and reported to yield a steeper temperature gradient at the liquid–solid [...] Read more.
This review describes the recent progress of floating-zone techniques for bulk single-crystal growth. The most crucial point of the crucible-free technique is to keep the molten zone stable. It has been investigated and reported to yield a steeper temperature gradient at the liquid–solid interface along the growth direction and a homogeneous molten liquid along the rotation axis. This article overviews several recent achievements starting from the conventional setup, particularly for lamps equipped in horizontal or vertical configurations, tilting mirrors, shielding the irradiation, and filament sizes for the optical-lamp floating-zone furnaces. Also, the recently advancing laser-heated floating-zone furnaces are described. Throughout the article, the author emphasizes that the floating-zone technique has been a powerful tool for crystal growth since the 1950s with its roots in the zone-melting method, and it has still been advancing for further materials’ growth such as quantum materials with modern scientific concepts. Full article
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