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Crystals, Volume 7, Issue 1 (January 2017)

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Cover Story (view full-size image) KSbTeO6 exhibits a defect pyrochlore structure defined in the cubic Fd3m symmetry. The mainly [...] Read more.
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Open AccessArticle Synthesis, Crystal Structure and DFT Studies of 1,3-Dimethyl-5-propionylpyrimidine-2,4,6(1H,3H,5H)-trione
Crystals 2017, 7(1), 31; https://doi.org/10.3390/cryst7010031
Received: 17 December 2016 / Revised: 12 January 2017 / Accepted: 16 January 2017 / Published: 21 January 2017
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Abstract
Novel 1,3-Dimethyl-5-propionylpyrimidine-2,4,6(1H,3H,5H)-trione was synthesized and recrystallized from ethanol. The compound was characterized by 1H NMR, 13C NMR in CDCl3, DMSO-d6 and acetone-d6, elemental analysis and X-ray diffraction. The
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Novel 1,3-Dimethyl-5-propionylpyrimidine-2,4,6(1H,3H,5H)-trione was synthesized and recrystallized from ethanol. The compound was characterized by 1H NMR, 13C NMR in CDCl3, DMSO-d6 and acetone-d6, elemental analysis and X-ray diffraction. The NMR data observed that the title compound exists in the enol tautomer rather than keto, and it stabilized by strong H-bond as observed form the NMR data at different temperatures. Theoretical calculations (DFT) were carried out using Gaussian09 program package and B3LYP correlation function. Full geometry optimization of the keto and enol forms were carried out using 6-311G++(d,p) basis set. The structure and energy of the transition state between these two tautomers were calculated. The frontier orbital energy and atomic net atomic charges of the tautomers were presented. The experimental results of the title compound have been compared with the theoretical results and it was found that the experimental data are in a good agreement with the calculated values. The transition state calculations also support the stability of enol form compared to keto form at room temperature. Full article
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Open AccessArticle Synthesis, Crystal Structure, Luminescence and Magnetism of Three Novel Coordination Polymers Based on Flexible Multicarboxylate Zwitterionic Ligand
Crystals 2017, 7(1), 32; https://doi.org/10.3390/cryst7010032
Received: 15 December 2016 / Revised: 12 January 2017 / Accepted: 16 January 2017 / Published: 20 January 2017
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Abstract
Three novel zwitterionic coordination polymers, namely, {[Zn(HCbdcp)2]·H2O} (1), {[Mn(Cbdcp)]·3H2O} (2) and {[Cu2(Cbdcp)(HCbdcp)Cl·H2O]·2H2O} (3), Cbdcp = 3,5-dicarboxy-1-(4-carboxybenzyl)pyridin-1-ium, have been prepared by a hydrothermal method and characterized
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Three novel zwitterionic coordination polymers, namely, {[Zn(HCbdcp)2]·H2O} (1), {[Mn(Cbdcp)]·3H2O} (2) and {[Cu2(Cbdcp)(HCbdcp)Cl·H2O]·2H2O} (3), Cbdcp = 3,5-dicarboxy-1-(4-carboxybenzyl)pyridin-1-ium, have been prepared by a hydrothermal method and characterized by X-ray single crystal diffraction analysis, powder X-ray diffraction analysis, IR spectroscopy, and thermogravimetric analysis. With the changing of metal centers, these complexes show distinct structures: a mononuclear 2D 44-sql network for 1, a 3D 6,6-connected-type topology for 2 and a novel dinuclear 2D layer for 3. These diverse architectures prove that coordination geometry of metal ions, coordination modes of carboxylate groups and the rotationally flexible CH2 linker played significant roles in the construction of CPs; moreover, they also indicated that H3CbdcpCl is an ideal organic candidate for the building of novel structures. The solid-state luminescent properties of complexes 13 were investigated, respectively. In addition, the magnetic properties of 2 and 3 were studied and both of them exhibit antiferromagnetic behaviors. Full article
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Open AccessArticle Colloidal Nanocrystalline Semiconductor Materials as Photocatalysts for Environmental Protection of Architectural Stone
Crystals 2017, 7(1), 30; https://doi.org/10.3390/cryst7010030
Received: 2 November 2016 / Revised: 23 December 2016 / Accepted: 14 January 2017 / Published: 20 January 2017
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Abstract
Rod-shaped TiO2 nanocrystals (TiO2 NRs), capped by oleic acid molecules (OLEA), were synthesized with controlled size, shape and surface chemistry by using colloidal routes. They were investigated for application as coating materials for preserving architectural stone of monumental and archaeological interest,
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Rod-shaped TiO2 nanocrystals (TiO2 NRs), capped by oleic acid molecules (OLEA), were synthesized with controlled size, shape and surface chemistry by using colloidal routes. They were investigated for application as coating materials for preserving architectural stone of monumental and archaeological interest, in consideration of their self-cleaning and protection properties. For this purpose, two different deposition techniques, namely casting and dipping, were tested for the application of a nanocrystal dispersion on a defined stone type, as a relevant example of porous calcarenites, namely the Pietra Leccese, a building stone widely used in monuments and buildings of cultural and historic interest of the Apulia region (Italy). The physical properties of the stone surface were investigated before and after the treatment with the prepared nanostructured materials. In particular, colour, wettability, water transfer properties and stability of the coating were monitored as a function of time and of the application method. The self-cleaning properties of the TiO2 NRs coated surfaces were tested under simulated and real solar irradiation. The obtained results were discussed in the light of the specific surface chemistry and morphology of TiO2 NRs, demonstrating the effectiveness of TiO2 NRs as an active component in formulations for stone protection. Full article
(This article belongs to the Special Issue Colloidal Nanocrystals: Synthesis, Characterization and Application)
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Open AccessReview Dirac Landau Level Spectroscopy in Pb1−xSnxSe and Pb1−xSnxTe across the Topological Phase Transition: A Review
Crystals 2017, 7(1), 29; https://doi.org/10.3390/cryst7010029
Received: 15 December 2016 / Revised: 7 January 2017 / Accepted: 7 January 2017 / Published: 20 January 2017
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Abstract
Topological crystalline insulators (TCIs) are topological materials that have Dirac surface states occurring at crystalline symmetric points in the Brillouin zone. This topological state has been experimentally shown to occur in the lead–tin salts Pb1−xSnxSe and Pb1−xSn
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Topological crystalline insulators (TCIs) are topological materials that have Dirac surface states occurring at crystalline symmetric points in the Brillouin zone. This topological state has been experimentally shown to occur in the lead–tin salts Pb1−xSnxSe and Pb1−xSnxTe. More recent works also took interest in studying the topological phase transition from trivial to non-trivial topology that occurs in such materials as a function of increasing Sn content. A peculiar property of these materials is the fact that their bulk bands disperse following a massive Dirac dispersion that is linear at low energies above the energy gap. This makes Pb1−xSnxSe and Pb1−xSnxTe ideal platforms to simultaneously study 3D and 2D Dirac physics. In this review, we will go over infrared magneto-optical studies of the Landau level dispersion of Pb1−xSnxSe and Pb1−xSnxTe for both the bulk and surface bands and summarize work that has been done on this matter. We will review recent work on probing the topological phase transition in TCI. We will finally present our views on prospects and open questions that have yet to be addressed in magneto-optical spectroscopy studies on Pb1-xSnxSe and Pb1−xSnxTe. Full article
(This article belongs to the Special Issue Topological Crystalline Insulators: Current Progress and Prospects)
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Open AccessArticle Ionic Liquid Crystals Modifier for Selective Determination of Terazosin Antihypertensive Drug in Presence of Common Interference Compounds
Crystals 2017, 7(1), 27; https://doi.org/10.3390/cryst7010027
Received: 30 November 2016 / Revised: 1 January 2017 / Accepted: 12 January 2017 / Published: 20 January 2017
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Abstract
Electrochemical sensor was fabricated based on carbon paste electrode modified with an ionic liquid crystal ILC (2-chloro-1,3-dimethyl-imidazolidinium hexafluorophosphate) in presence of sodium dodecyl sulfate for the selective electrochemical determination of Terazosin (TZ) in presence of common interference compounds. The electrode performance was compared
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Electrochemical sensor was fabricated based on carbon paste electrode modified with an ionic liquid crystal ILC (2-chloro-1,3-dimethyl-imidazolidinium hexafluorophosphate) in presence of sodium dodecyl sulfate for the selective electrochemical determination of Terazosin (TZ) in presence of common interference compounds. The electrode performance was compared in presence of other ionic liquids ILs (1-Butyl-4-methyl pyridinium tetrafluoroborate) and (1-n-Hexyl-3-methyl imidazolium tetrafluoroborate). Ultrasensitive determination of Terazosin HCl at the ILC modified electrode in the linear dynamic ranges of 0.002 to 0.09 μmol·L−1 and 0.2 to 30 μmol·L−1 with correlation coefficients 0.996 and 0.995 and LODs 1.69 × 10−11 mol·L−1 and 6.43 × 10−9 mol·L−1, respectively, were obtained. Selective determination of TZ in presence of uric acid and ascorbic acid and simultaneous determination of binary mixtures of TZ/dopamine, TZ/paracetamol and TZ/Morphine were also determined successfully using the modified sensor. Full article
(This article belongs to the Section Liquid Crystals)
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Open AccessArticle The New Method of XRD Measurement of the Degree of Disorder for Anode Coke Material
Crystals 2017, 7(1), 5; https://doi.org/10.3390/cryst7010005
Received: 6 November 2016 / Revised: 22 December 2016 / Accepted: 24 December 2016 / Published: 18 January 2017
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Abstract
Quantitative analysis by X-ray powder diffraction of two cokes (pitch coke and petroleum coke) shows that their crystal structure changed with increasing temperature. The crystal data processing of the crystallization degree of disorder is used with further improvement of the proposed microcrystalline-stacking fault
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Quantitative analysis by X-ray powder diffraction of two cokes (pitch coke and petroleum coke) shows that their crystal structure changed with increasing temperature. The crystal data processing of the crystallization degree of disorder is used with further improvement of the proposed microcrystalline-stacking fault calculation method. With this improvement it is now possible to obtain the degree of stacking disorder of two cokes applied as anode materials at different graphitization temperatures. Raman spectroscopy verified the accuracy of this method, which is more reliable than the crystal structure refinement using the d002 method. This paper provides the theoretical analysis and interpretation of the relationship between the microstructure model of the material and quantitative data, discharge capacity, and the first charge-discharge efficiency. Full article
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Open AccessArticle Influence of Alkyl Trimethyl Ammonium Bromides on Hydrothermal Formation of α-CaSO4·0.5H2O Whiskers with High Aspect Ratios
Crystals 2017, 7(1), 28; https://doi.org/10.3390/cryst7010028
Received: 1 December 2016 / Revised: 11 January 2017 / Accepted: 16 January 2017 / Published: 18 January 2017
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Abstract
In this paper, the influence of alkyl trimethyl ammonium bromides (CnH2n+1(CH3)3NBr, n = 10, 12, 14, 16, 18, abbreviated as ATAB) on the formation of alpha calcium sulfate hemihydrate (α-CaSO4·0.5H2O) whiskers
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In this paper, the influence of alkyl trimethyl ammonium bromides (CnH2n+1(CH3)3NBr, n = 10, 12, 14, 16, 18, abbreviated as ATAB) on the formation of alpha calcium sulfate hemihydrate (α-CaSO4·0.5H2O) whiskers under a hydrothermal condition (135 °C, 3.0 h) was analyzed. Specifically, it focuses on cetyl trimethyl ammonium bromide (C16H33(CH3)3NBr, abbreviated as CTAB). The rising CTAB concentration from 0 to 9.2 × 10−4 mol·L−1 led to the increase of the average aspect ratio of α-CaSO4·0.5H2O whiskers from 80 to 430, since the selective adsorption of CTAB on the negatively-charged side facets of the whiskers inhibited the growth of the whiskers along the direction normal to the lateral facets. The further increase of CTAB concentration above the critical micelle concentration (abbreviated as CMC) showed little effect on the morphology of α-CaSO4·0.5H2O whiskers, considering that CTAB tended to form micelles instead of being adsorbed on the whisker surfaces. Similar phenomena were observed in other ATABs (n = 10, 12, 14, 18). Full article
(This article belongs to the Special Issue Solution-Processed Inorganic Functional Crystals)
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Open AccessArticle Numerical Modelling of the Czochralski Growth of β-Ga2O3
Crystals 2017, 7(1), 26; https://doi.org/10.3390/cryst7010026
Received: 25 November 2016 / Revised: 3 January 2017 / Accepted: 6 January 2017 / Published: 17 January 2017
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Abstract
Our numerical modelling of the Czochralski growth of single crystalline β-Ga2O3 crystals (monoclinic symmetry) starts at the 2D heat transport analysis within the crystal growth furnace, proceeds with the 3D heat transport and fluid flow analysis in the crystal-melt-crucible
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Our numerical modelling of the Czochralski growth of single crystalline β-Ga 2 O 3 crystals (monoclinic symmetry) starts at the 2D heat transport analysis within the crystal growth furnace, proceeds with the 3D heat transport and fluid flow analysis in the crystal-melt-crucible arrangement and targets the 3D thermal stress analysis within the β-Ga 2 O 3 crystal. In order to perform the stress analysis, we measured the thermal expansion coefficients and the elastic stiffness coefficients in two samples of a β-Ga 2 O 3 crystal grown at IKZ. Additionally, we analyse published data of β-Ga 2 O 3 material properties and use data from literature for comparative calculations. The computations were performed by the software packages CrysMAS, CGsim, Ansys-cfx and comsol Multiphysics. By the hand of two different thermal expansion data sets and two different crystal orientations, we analyse the elastic stresses in terms of the von-Mises stress. Full article
(This article belongs to the Special Issue Global Modeling in Crystal Growth)
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Open AccessArticle Four Thermochromic o-Hydroxy Schiff Bases of α-Aminodiphenylmethane: Solution and Solid State Study
Crystals 2017, 7(1), 25; https://doi.org/10.3390/cryst7010025
Received: 15 December 2016 / Revised: 9 January 2017 / Accepted: 11 January 2017 / Published: 14 January 2017
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Abstract
More than a hundred years after the first studies of the photo- and thermochromism of o-hydroxy Schiff bases (imines), it is still an intriguing topic that fascinates several research groups around the world. The reasons for such behavior are still under investigation,
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More than a hundred years after the first studies of the photo- and thermochromism of o-hydroxy Schiff bases (imines), it is still an intriguing topic that fascinates several research groups around the world. The reasons for such behavior are still under investigation, and this work is a part of it. We report the solution-based and mechanochemical synthesis of four o-hydroxy imines derived from α-aminodiphenylmethane. The thermochromic properties were studied for the single crystal and polycrystalline samples of the imines. The supramolecular impact on the keto-enol tautomerism in the solid state was studied using SCXRD and NMR, while NMR spectroscopy was used for the solution state. All four imines are thermochromic, although the color changes of the single crystals are not as strong as of the polycrystalline samples. One of the imines shows negative thermochromism, and that one is in keto-amine tautomeric form, both in the solid state as in solution. Full article
(This article belongs to the Special Issue Thermo- and Photochromic Molecular Crystals)
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Open AccessArticle Potassium Disorder in the Defect Pyrochlore KSbTeO6: A Neutron Diffraction Study
Crystals 2017, 7(1), 24; https://doi.org/10.3390/cryst7010024
Received: 25 November 2016 / Revised: 13 December 2016 / Accepted: 26 December 2016 / Published: 13 January 2017
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Abstract
KSbTeO6 defect pyrochlore has been prepared from K2C2O4, Sb2O3, and 15% excess TeO2 by solid-state reaction at 850 °C. Direct methods implemented in the software EXPO2013 allowed establishing the basic structural
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KSbTeO6 defect pyrochlore has been prepared from K2C2O4, Sb2O3, and 15% excess TeO2 by solid-state reaction at 850 °C. Direct methods implemented in the software EXPO2013 allowed establishing the basic structural framework. This was followed by a combined Rietveld refinement from X-ray powder diffraction (XRD) and neutron powder diffraction (NPD) data, which unveiled additional structural features. KSbTeO6 is cubic, a = 10.1226(7) Å, space group F d 3 ¯ m , Z = 8 and it is made of a mainly covalent framework of corner-sharing (Sb,Te)O6 octahedra, with weakly bonded K+ ions located within large cages. The large K-O distances, 3.05(3)–3.07(3) Å, and quite large anisotropic atomic displacement parameters account for the easiness of K+ exchange for other cations of technological importance. Full article
(This article belongs to the Special Issue Structural Analysis of Crystalline Materials from Powders)
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Open AccessArticle Synthesizing Iron Oxide Nanostructures: The Polyethylenenemine (PEI) Role
Crystals 2017, 7(1), 22; https://doi.org/10.3390/cryst7010022
Received: 23 November 2016 / Revised: 6 January 2017 / Accepted: 9 January 2017 / Published: 12 January 2017
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Abstract
Controlled synthesis of anisotropic iron oxide nanoparticles is a challenge in the field of nanomaterial research that requires an extreme attention to detail. In particular, following up a previous work showcasing the synthesis of magnetite nanorods (NRs) using a two-step approach that made
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Controlled synthesis of anisotropic iron oxide nanoparticles is a challenge in the field of nanomaterial research that requires an extreme attention to detail. In particular, following up a previous work showcasing the synthesis of magnetite nanorods (NRs) using a two-step approach that made use of polyethylenenemine (PEI) as a capping ligand to synthesize intermediate β-FeOOH NRs, we studied the effect and influence of the capping ligand on the formation of β-FeOOH NRs. By comparing the results reported in the literature with those we obtained from syntheses performed (1) in the absence of PEI or (2) by using PEIs with different molecular weight, we showed how the choice of different PEIs determines the aspect ratio and the structural stability of the β-FeOOH NRs and how this affects the final products. For this purpose, a combination of XRD, HRTEM, and direct current superconducting quantum interference device (DC SQUID) magnetometry was used to identify the phases formed in the final products and study their morphostructural features and related magnetic behavior. Full article
(This article belongs to the Special Issue Colloidal Nanocrystals: Synthesis, Characterization and Application)
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Open AccessEditorial Crystal Indentation Hardness
Crystals 2017, 7(1), 21; https://doi.org/10.3390/cryst7010021
Received: 5 January 2017 / Accepted: 6 January 2017 / Published: 12 January 2017
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Abstract
There is expanded interest in the long-standing subject of the hardness properties of materials. A major part of such interest is due to the advent of nanoindentation hardness testing systems which have made available orders of magnitude increases in load and displacement measuring
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There is expanded interest in the long-standing subject of the hardness properties of materials. A major part of such interest is due to the advent of nanoindentation hardness testing systems which have made available orders of magnitude increases in load and displacement measuring capabilities achieved in a continuously recorded test procedure. The new results have been smoothly merged with other advances in conventional hardness testing and with parallel developments in improved model descriptions of both elastic contact mechanics and dislocation mechanisms operative in the understanding of crystal plasticity and fracturing behaviors. No crystal is either too soft or too hard to prevent the determination of its elastic, plastic and cracking properties under a suitable probing indenter. A sampling of the wealth of measurements and reported analyses associated with the topic on a wide variety of materials are presented in the current Special Issue. Full article
(This article belongs to the Special Issue Crystal Indentation Hardness) Printed Edition available
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Open AccessArticle Synthesis, Crystal Structure, DFT Study of m-Methoxy-N′-(3-Methoxybenzoyl)-N-Phenylbenzohydrazide
Crystals 2017, 7(1), 19; https://doi.org/10.3390/cryst7010019
Received: 19 August 2016 / Revised: 4 January 2017 / Accepted: 5 January 2017 / Published: 12 January 2017
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Abstract
The crystal structure of m-methoxy-N′-(m-anisoyl)-N-phenylbenzohydrazide has been determined by means of single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic space group P 21/c with unit cell parameters: a = 8.7338(1), b = 24.5602(3), c
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The crystal structure of m-methoxy-N′-(m-anisoyl)-N-phenylbenzohydrazide has been determined by means of single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic space group P 21/c with unit cell parameters: a = 8.7338(1), b = 24.5602(3), c = 9.6929(1) Å, β = 113.186(2)°, V = 1911.23(4) Å3, Z = 4. The dihedral angles between the mean plane of the central benzene ring and two terminal aromatic rings are 72.44(4)° and 89.90(4)°, respectively. The two methoxyphenyl rings are orthogonal with a dihedral angle of 89.74(4)°. The crystal packing is stabilized by a combination of N–HO intermolecular hydrogen bonding and weak intermolecular C–HO interactions. The X-ray structure was compared with the optimized counterpart calculated by the B3LYP/6-311G basis set and the results showed that the optimized geometry can reproduce the crystal structure parameters well. Full article
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Open AccessEditorial Acknowledgement to Reviewers of Crystals in 2016
Crystals 2017, 7(1), 20; https://doi.org/10.3390/cryst7010020
Received: 11 January 2017 / Revised: 11 January 2017 / Accepted: 11 January 2017 / Published: 11 January 2017
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Abstract
The editors of Crystals would like to express their sincere gratitude to the following reviewers for assessing manuscripts in 2016.[...] Full article
Open AccessArticle Role of Internal Radiation in Oxide Crystal Growth by Heat Exchanger Method
Crystals 2017, 7(1), 18; https://doi.org/10.3390/cryst7010018
Received: 18 October 2016 / Revised: 21 December 2016 / Accepted: 5 January 2017 / Published: 9 January 2017
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Abstract
Internal radiation was investigated using the finite volume method for the heat exchanger method (HEM) growth of oxide crystals. Special attention was devoted to the temperature and thermal stress distributions in the bottom region of the grown crystal at the end of the
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Internal radiation was investigated using the finite volume method for the heat exchanger method (HEM) growth of oxide crystals. Special attention was devoted to the temperature and thermal stress distributions in the bottom region of the grown crystal at the end of the solidification process. The numerical results show that internal radiation strongly strengthens heat transport through the crystal. However, it causes isotherms to intensively concentrate in the crystal bottom region, leading to a significant increase in the temperature gradient and thermal stress in this region. Then, the effect of absorption coefficient on this phenomenon was numerically investigated. It was found that the radiation heat transfer rate at the bottom surface of the crystal monotonically decreases as the absorption coefficient is increased, while the conduction heat transfer rate first increases and then decreases as the absorption coefficient is increased, under the interaction between internal radiation and heat conduction. The variations of the maximum temperature gradient and thermal stress in the crystal bottom show the same tendency as the conduction heat transfer rate. This study indicates that the role of internal radiation on the heat transfer and thermal stress in oxide crystal by HEM process shows some differences from that by Czochralski and Kyropoulos processes. Full article
(This article belongs to the Special Issue Global Modeling in Crystal Growth)
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