Crystallization Process and Simulation Calculation

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

Deadline for manuscript submissions: closed (30 April 2023) | Viewed by 24878

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Special Issue Editors

State Key Laboratory of Chemical Engineering, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China
Interests: crystallization process; spherical crystallization; nucleation; crystal growth; crystal agglomeration; simulation; particle engineering
Special Issues, Collections and Topics in MDPI journals
School of Chemistry, Biology and Materials Science, East China University of Technology, Nanchang 330013, China
Interests: polymorph nucleation; template-assisted crystallization; cocrystallizaiton design; porous biochar composites
Special Issues, Collections and Topics in MDPI journals
State Key Laboratory of Chemical Engineering, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China
Interests: industrial crystallization; crystal engineering; crystal habit engineering; nucleation; crystal growth; molecular dynamics

Special Issue Information

Dear Colleagues,

As an important unit operation, crystallization is a process in which nucleation, growth, agglomeration, and breakage are regulated to produce high-quality crystals and achieve efficient separation as well as purification. In recent years, there have been some new research developments in crystallization processes. Process intensification techniques such as ultrasound and wet grinding are used to enhance the nucleation and breakage processes in crystallization, thereby preparing ultrafine powders and cube-like crystals. Spherical crystallization technology prepares spherical crystalline particles through crystal growth or agglomeration processes. Continuous crystallization has also gained growing interest due to its high productivity and consistency of the product quality. These studies could provide innovative process design strategies and control methods for crystallizing a product with requisite quality attributes and predictable performance. Since a crystallization process often presents the characteristics of strong coupling, nonlinearity, and large lagging, it is a challenge to rationally design a robust, well-characterized process to efficiently crystallize and prepare a high-quality crystalline product. The development of process analytical technology that can provide fast and accurate inline or online measurement is of great importance in the design and control of crystallization processes. Simulation technology, e.g., molecular dynamics simulation and hydrodynamics simulation, can provide a time- or location-dependent insight into the process on multiple scales. These experimental and simulation tools can greatly help to further investigate crystallization processes.

This Special Issue, “Crystallization Process and Simulation Calculation”, serves to provide a platform for researchers to report results and findings in crystallization process technologies, simulation and process analytical technologies, and relevant crystallization studies.

Dr. Mingyang Chen
Dr. Jinbo Ouyang
Dr. Dandan Han
Guest Editors

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Keywords

  • nucleation and growth
  • agglomeration and breakage
  • process analytical technology
  • process intensification
  • continuous crystallization
  • spherical crystallization
  • molecular dynamics simulation
  • hydrodynamics simulation

Published Papers (12 papers)

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Research

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12 pages, 2949 KiB  
Article
The Influence of Hydrothermal Temperature on Alumina Hydrate and Ammonioalunite Synthesis by Reaction Crystallization
by Junkai Wang, Laishi Li, Yusheng Wu and Yuzheng Wang
Crystals 2023, 13(5), 763; https://doi.org/10.3390/cryst13050763 - 04 May 2023
Viewed by 1222
Abstract
With the rapid development of the alumina industry and the shortage of bauxite, high-alumina coal fly ash (HACFA) has attracted more and more attention as a potential alternative alumina resource. In order to extract alumina from HACFA with newly developed technology, the investigation [...] Read more.
With the rapid development of the alumina industry and the shortage of bauxite, high-alumina coal fly ash (HACFA) has attracted more and more attention as a potential alternative alumina resource. In order to extract alumina from HACFA with newly developed technology, the investigation of the crucial step, the reaction between NH4Al(SO4)2·12H2O and NH3·H2O, is necessary and valuable. Thermodynamic analyses have shown that four kinds of alumina hydrate (boehmite, diaspore, gibbsite, and bayerite) might be formed at 120–200 °C, and ammonioalunite might be formed at temperatures over 180 °C. A hydrothermal reaction crystallization method was applied to this reaction. The experimental results showed that boehmite (AlOOH) could be formed at 150 °C and 200 °C after 12 h and NH4Al3(SO4)2(OH)6, an unstable intermediate, is formed during the initial stage and transformed into boehmite, eventually. The higher temperature (200 °C) was more energetically favorable for the formation of NH4Al3(SO4)2(OH)6, and the crystallinity of the products was better. More importantly, the sheet-like structure of boehmite (AlOOH) could be formed at 150 °C after 24 h of reaction time. The SEM results proved that the sheet-like structures evolutionary process of boehmite. Full article
(This article belongs to the Special Issue Crystallization Process and Simulation Calculation)
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15 pages, 2992 KiB  
Article
Optimizing Struvite Crystallization at High Stirring Rates
by Atef Korchef, Salwa Abouda and Imen Souid
Crystals 2023, 13(4), 711; https://doi.org/10.3390/cryst13040711 - 21 Apr 2023
Cited by 3 | Viewed by 1434
Abstract
Phosphorus and ammonium can both be recovered in the presence of magnesium through struvite (MgNH4PO4·6H2O) crystallization. The present work aimed to optimize struvite crystallization at turbulent solution flow. Struvite was crystallized by magnetic stirring at different initial [...] Read more.
Phosphorus and ammonium can both be recovered in the presence of magnesium through struvite (MgNH4PO4·6H2O) crystallization. The present work aimed to optimize struvite crystallization at turbulent solution flow. Struvite was crystallized by magnetic stirring at different initial phosphorus concentrations between 200 and 800 mg·L−1 and high stirring rates between 100 and 700 rpm. The crystals obtained were analyzed by powder X-ray diffraction, Fourier-transform infrared spectroscopy, and scanning electron microscopy. For all experiments, the only phase detected was struvite. It was shown that for an initial phosphorus concentration of 200 mg·L−1, increasing the stirring rate to 500 rpm accelerated the precipitation of struvite, improved the phosphorus removal efficiency, and obtained larger struvite crystals. A decrease in the phosphorus removal efficiency and smaller struvite crystals were obtained at higher stirring rates. This was attributed to the solution turbulence. The limiting effect of turbulence could be overcome by enhancing the initial phosphorus concentration or by lowering the stirring rate. The highest phosphorus removal efficiency (~99%) through large struvite crystals (~400 μm in size) was obtained for an initial phosphorus concentration of 800 mg·L−1 and a stirring rate of 100 rpm. Full article
(This article belongs to the Special Issue Crystallization Process and Simulation Calculation)
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15 pages, 4743 KiB  
Article
Influence of Foreign Salts and Antiscalants on Calcium Carbonate Crystallization
by Raghda Hamdi and Mohamed Mouldi Tlili
Crystals 2023, 13(3), 516; https://doi.org/10.3390/cryst13030516 - 17 Mar 2023
Viewed by 1077
Abstract
For more than a century, crystallization has remained a chief research topic. One of the most undesirable crystallization phenomena is the formation of calcium carbonate scale in drinking and industrial water systems. In this work, the influence of chemical additives on CaCO3 [...] Read more.
For more than a century, crystallization has remained a chief research topic. One of the most undesirable crystallization phenomena is the formation of calcium carbonate scale in drinking and industrial water systems. In this work, the influence of chemical additives on CaCO3 formation—in either nucleation, crystal growth, or inhibition processes—is investigated by using the CO2-degasification method. Chemical additives are foreign salts (MgCl2, Na2SO4 and MgSO4) to the calco-carbonic system and antiscalants (sodium polyacrylate ‘RPI’ and sodium-tripolyphosphate ‘STPP’). The results show that additives affects both crystallization kinetics and the CaCO3 microstructure. Sulfate and magnesium ions, added separately at constant ionic strength, influence the nucleation step more than the growth of the formed crystallites. Added simultaneously, their effect was accentuated on both nucleation and the growth of CaCO3. Furthermore, antiscalants RPI and STPP affect the crystallization process by greatly delaying the precipitation time and largely increasing the supersaturation coefficient. It was also shown that the calco-carbonic system with additives prefers the heterogeneous nucleation to the homogeneous one. X-ray diffraction patterns show that additives promote the formation of a new crystal polymorph of calcium carbonate as aragonite, in addition to the initial polymorphs formed as calcite and vaterite. Full article
(This article belongs to the Special Issue Crystallization Process and Simulation Calculation)
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13 pages, 3709 KiB  
Article
Long-Term Stability of Novel Crucible Systems for the Growth of Oxygen-Free Czochralski Silicon Crystals
by Felix Sturm, Matthias Trempa, Gordian Schuster, Rainer Hegermann, Philipp Goetz, Rolf Wagner, Gilvan Barroso, Patrick Meisner, Christian Reimann and Jochen Friedrich
Crystals 2023, 13(1), 14; https://doi.org/10.3390/cryst13010014 - 22 Dec 2022
Cited by 1 | Viewed by 1828
Abstract
The replacement of the silica glass crucible by oxygen-free crucible materials in silicon Czochralski (Cz) growth technology could be a key factor to obtaining Cz silicon, with extremely low oxygen contamination < 1 × 1017 at/cm3 required for power electronic applications. [...] Read more.
The replacement of the silica glass crucible by oxygen-free crucible materials in silicon Czochralski (Cz) growth technology could be a key factor to obtaining Cz silicon, with extremely low oxygen contamination < 1 × 1017 at/cm3 required for power electronic applications. So far, isostatic pressed graphite or nitrogen-bonded silicon nitride (NSN) crucible material, in combination with a chemical vapor deposited silicon nitride (CVD-Si3N4) surface coating, could be identified as promising materials by first short-term experiments. However, for the evaluation of their potential for industrial scale Cz growth application, the knowledge about the long-term behavior of these crucible setups is mandatory. For that purpose, the different materials were brought in contact with silicon melt up to 60 h to investigate the infiltration and dissolution behavior. The chosen graphite, as well as the pore-sealed NSN material, revealed a subordinated infiltration-depth of ≤1 mm and dissolution of ≤275 µm by the silicon melt, so they basically fulfilled the general safety requirements for Cz application. Further, the highly pure and dense CVD Si3N4 crucible coating showed no measurable infiltration as well as minor dissolution of ≤50 µm and may further acts as a nucleation site for nitrogen-based precipitates. Consequently, these novel crucible systems have a high potential to withstand the stresses during industrial Cz growth considering that more research on the process side relating to the particle transport in the silicon melt is needed. Full article
(This article belongs to the Special Issue Crystallization Process and Simulation Calculation)
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20 pages, 4757 KiB  
Article
Numerical Simulation of Species Segregation and 2D Distribution in the Floating Zone Silicon Crystals
by Kirils Surovovs, Maksims Surovovs, Andrejs Sabanskis, Jānis Virbulis, Kaspars Dadzis, Robert Menzel and Nikolay Abrosimov
Crystals 2022, 12(12), 1718; https://doi.org/10.3390/cryst12121718 - 26 Nov 2022
Cited by 1 | Viewed by 2079
Abstract
The distribution of dopants and impurities in silicon grown with the floating zone method determines the electrical resistivity and other important properties of the crystals. A crucial process that defines the transport of these species is the segregation at the crystallization interface. To [...] Read more.
The distribution of dopants and impurities in silicon grown with the floating zone method determines the electrical resistivity and other important properties of the crystals. A crucial process that defines the transport of these species is the segregation at the crystallization interface. To investigate the influence of the melt flow on the effective segregation coefficient as well as on the global species transport and the resulting distribution in the grown crystal, we developed a new coupled numerical model. Our simulation results include the shape of phase boundaries, melt flow velocity and temperature, species distribution in the melt and, finally, the radial and axial distributions in the grown crystal. We concluded that the effective segregation coefficient is not constant during the growth process but rather increases for larger melt diameters due to less intensive melt mixing. Full article
(This article belongs to the Special Issue Crystallization Process and Simulation Calculation)
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11 pages, 2767 KiB  
Article
Image Measurement of Crystal Size Growth during Cooling Crystallization Using High-Speed Imaging and a U-Net Network
by Yan Huo, Xin Li and Binbin Tu
Crystals 2022, 12(12), 1690; https://doi.org/10.3390/cryst12121690 - 22 Nov 2022
Cited by 1 | Viewed by 1539
Abstract
In this paper, an image measurement method using a high-speed imaging system is proposed for the evolution of crystal population sizes during cooling crystallization processes. Firstly, to resist the negative effect from solution stirring and particle motion during crystallization, a U-net network-based image [...] Read more.
In this paper, an image measurement method using a high-speed imaging system is proposed for the evolution of crystal population sizes during cooling crystallization processes. Firstly, to resist the negative effect from solution stirring and particle motion during crystallization, a U-net network-based image processing method is established to efficiently detect sufficiently clear crystals from the online captured microscopic images. Accordingly, the crystal size distribution model is analyzed in terms of the counted probability densities of these crystal images. Subsequently, a measurement method of size growth rate based on crystal population distribution is proposed to estimate the growth condition. An experimental case on a crystallization process of β-form LGA is used to show the effectiveness of the proposed strategy. Full article
(This article belongs to the Special Issue Crystallization Process and Simulation Calculation)
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9 pages, 1896 KiB  
Article
Sn-Doped Hydrated V2O5 Cathode Material with Enhanced Rate and Cycling Properties for Zinc-Ion Batteries
by Kai Guo, Wenchong Cheng, Haiyuan Liu, Wenhao She, Yinpeng Wan, Heng Wang, Hanbin Li, Zidan Li, Xing Zhong, Jinbo Ouyang and Neng Yu
Crystals 2022, 12(11), 1617; https://doi.org/10.3390/cryst12111617 - 11 Nov 2022
Cited by 2 | Viewed by 1493
Abstract
Water molecules and cations with mono, binary, and triple valences have been intercalated into V2O5 to significantly improve its electrochemical properties as a cathode material of zinc-ion batteries. Sn as a tetravalent element is supposed to interact aggressively with the [...] Read more.
Water molecules and cations with mono, binary, and triple valences have been intercalated into V2O5 to significantly improve its electrochemical properties as a cathode material of zinc-ion batteries. Sn as a tetravalent element is supposed to interact aggressively with the V2O5 layer and have a significant impact on the electrochemical performance of V2O5. However, it has been rarely investigated as a pre-intercalated ion in previous works. Hence, it is intriguing and beneficial to develop water molecules and Sn co-doped V2O5 for zinc-ion batteries. Herein, Sn-doped hydrated V2O5 nanosheets were prepared by a one-step hydrothermal synthesis, and they demonstrated that they had a high specific capacity of 374 mAh/g at 100 mA/g. Meanwhile, they also showed an exceptional rate capability with 301 mAh/g even at a large current density of 10 A/g, while it was only 40 mAh/g for the pristine hydrated V2O5, and an excellent cycling life (87.2% after 2500 cycles at 5 A/g), which was far more than the 25% of the pure hydrated V2O5. The dramatic improvement of the rate and cycling performance is mainly attributed to the faster charge transfer kinetics and the enhanced crystalline framework. The remarkable electrochemical performance makes the Sn-doped hydrate V2O5 a potential cathode material for zinc-ion batteries. Full article
(This article belongs to the Special Issue Crystallization Process and Simulation Calculation)
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22 pages, 2737 KiB  
Article
Measurement and Correlation of the Solubility of Florfenicol in Four Binary Solvent Mixtures from T = (278.15 to 318.15) K
by Xinyuan Zhang, Pingping Cui, Qiuxiang Yin and Ling Zhou
Crystals 2022, 12(8), 1176; https://doi.org/10.3390/cryst12081176 - 21 Aug 2022
Cited by 1 | Viewed by 1696
Abstract
Florfenicol is an excellent antibiotic and is widely used in animal bacterial diseases. However, its poor water solubility leads to various problems, such as poor absorption and bioavailability. The development of nanocrystals is one of the most useful methods for solubilizing florfenicol, which [...] Read more.
Florfenicol is an excellent antibiotic and is widely used in animal bacterial diseases. However, its poor water solubility leads to various problems, such as poor absorption and bioavailability. The development of nanocrystals is one of the most useful methods for solubilizing florfenicol, which often requires solubility data of florfenicol in different mixed solvents. In this work, the solubility of florfenicol was determined by the gravimetric method in methanol + water, ethanol + water, 1-propanol + water, and isopropanol + water binary solvents at temperatures from 278.15 to 318.15 K. In these four mixed solvents, the solubility of florfenicol increased with the increase in temperature. The solubility of florfenicol in methanol + water mixed solvent increases with the decrease in water ratio, while the solubility of florfenicol in ethanol + water, 1-propanol + water, or isopropanol + water mixed solvents increased first and then decreased with the decrease in water ratio, indicating a cosolvency phenomenon. The modified Apelblat model, CNIBS/R-K model, Jouyban–Acree model, and NRTL model were used to correlate the solubility data of florfenicol in four binary solvents. RMSD values indicated that the calculated values are in good agreement with the experimental solubility data for all four models, among which the CNIBS/R-K model provides the best correlation. Full article
(This article belongs to the Special Issue Crystallization Process and Simulation Calculation)
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13 pages, 3632 KiB  
Article
Study on Deposition Conditions in Coupled Polysilicon CVD Furnaces by Simulations
by Shengtao Zhang, Hao Fu, Guofeng Fan, Tie Li, Jindou Han and Lili Zhao
Crystals 2022, 12(8), 1129; https://doi.org/10.3390/cryst12081129 - 12 Aug 2022
Cited by 1 | Viewed by 2232
Abstract
Electronic-grade polysilicon is the cornerstone of the information industry. Considering the demand for this material in the semiconductor industry, any technological improvement has great potential benefits. Due to the quality requirements of electronic polysilicon, its preparation process is characterized by low raw material [...] Read more.
Electronic-grade polysilicon is the cornerstone of the information industry. Considering the demand for this material in the semiconductor industry, any technological improvement has great potential benefits. Due to the quality requirements of electronic polysilicon, its preparation process is characterized by low raw material utilization and high cost. Simply increasing the deposition rate by increasing the chemical reaction rate will easily lead to a reduction in the proportion of dense materials. For the first time, a coupled furnace scheme is proposed to improve the utilization of raw materials while maintaining the same deposition quality. The deposition conditions on the surface of silicon rods with different base plate designs were modeled and analyzed using the software PolySim, and a design characterized by a high flow rate and the use of 9 mm and 15 mm nozzles was selected for the coupling scheme. In coupling mode, the simulation results show that the utilization of raw materials is increased by 17.5%, and the deposition rate is increased by 44.9%, while the deposition quality and uniformity remain approximately unchanged. The results show that the coupling scheme with high feed flow is beneficial for significantly improving the deposition conditions and the utilization rate of raw materials, which also provides guidance for material preparation processes with similar principles. Full article
(This article belongs to the Special Issue Crystallization Process and Simulation Calculation)
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8 pages, 1967 KiB  
Article
2D Layer Structure in Two New Cu(II) Crystals: Structural Evolvement and Properties
by Jia-Jing Luo, Xiang-Xin Cao, Qi-Wei Chen, Ying Qin, Zhen-Wei Zhang, Lian-Qiang Wei and Qing Chen
Crystals 2022, 12(5), 585; https://doi.org/10.3390/cryst12050585 - 22 Apr 2022
Viewed by 1175
Abstract
Two new Cu(II) crystals, {[Cu(dtp)]·H2O}n (1) and [Cu(Hdtp)(bdc)0.5]n (2) (H2dtp = 4′-(3,5-dicarboxyphenyl)-2,2′:6′,2‴-terpyridine, H2bdc = 1,4-benzenedicarboxylic acid) were synthesized under hydrothermal conditions. X-ray single-crystal structural analysis revealed that the 5-connective [...] Read more.
Two new Cu(II) crystals, {[Cu(dtp)]·H2O}n (1) and [Cu(Hdtp)(bdc)0.5]n (2) (H2dtp = 4′-(3,5-dicarboxyphenyl)-2,2′:6′,2‴-terpyridine, H2bdc = 1,4-benzenedicarboxylic acid) were synthesized under hydrothermal conditions. X-ray single-crystal structural analysis revealed that the 5-connective Cu(II) is in a distorted tetragonal-pyramidal coordination sphere for both compounds. Crystal 1 shows a “wave-shaped” 2D layer in the structure, while 2 bears a 1D coordination chain structure and a supermolecular 2D layer structure with a thickness of 7.9 Å via 1D chain stacking. PXRD and TGA measurements showed that 1 and 2 are air stable, with thermal stabilities near 300 °C. Full article
(This article belongs to the Special Issue Crystallization Process and Simulation Calculation)
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Review

Jump to: Research

22 pages, 4403 KiB  
Review
Research on Mesoscale Nucleation and Growth Processes in Solution Crystallization: A Review
by Xiaowei Wang, Kangli Li, Xueyou Qin, Mingxuan Li, Yanbo Liu, Yanlong An, Wulong Yang, Mingyang Chen, Jinbo Ouyang and Junbo Gong
Crystals 2022, 12(9), 1234; https://doi.org/10.3390/cryst12091234 - 01 Sep 2022
Cited by 4 | Viewed by 4440
Abstract
In recent studies, the existence of mesoscale precursors has been confirmed in crystallization. Different from the classical crystallization theory, which only considers the sequential attachment of basic monomers (atoms, ions, or molecules), the nonclassical crystallization process involving precursors such as prenucleation clusters, nanoparticles, [...] Read more.
In recent studies, the existence of mesoscale precursors has been confirmed in crystallization. Different from the classical crystallization theory, which only considers the sequential attachment of basic monomers (atoms, ions, or molecules), the nonclassical crystallization process involving precursors such as prenucleation clusters, nanoparticles, and mesocrystals is more complicated. The mesoscale structure is important for the quantitative description and directional regulation of the solution crystallization process. It is necessary to explore the mechanism by the mesoscale scientific research methods on the base of traditional chemical engineering and process system engineering research methods. Therefore, the paper reviews several representative nonclassical nucleation and growth theories, mainly including two-step nucleation theory, prenucleation clusters theory, particle agglomeration theory, amorphous precursor growth theory, particle attachment growth theory and mesocrystal growth theory. Then, the mesoscale structure and its spatiotemporal dynamic behavior are discussed, and the application of the EMMS model in the nucleation and growth process is analyzed. Finally, we put forward our views on the prospect of the paradigms and theoretical innovations of using mesoscale methods in crystal nucleation and growth. Full article
(This article belongs to the Special Issue Crystallization Process and Simulation Calculation)
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21 pages, 3338 KiB  
Review
Advances of Combinative Nanocrystal Preparation Technology for Improving the Insoluble Drug Solubility and Bioavailability
by Qiuyan Ran, Mengwei Wang, Wenjie Kuang, Jinbo Ouyang, Dandan Han, Zhenguo Gao and Junbo Gong
Crystals 2022, 12(9), 1200; https://doi.org/10.3390/cryst12091200 - 25 Aug 2022
Cited by 9 | Viewed by 3319
Abstract
The low solubility and bioavailability of aqueous insoluble drugs are critical challenges in the field of pharmaceuticals that need to be overcome. Nanocrystal technology, a novel pharmacological route to address the poor aqueous solubility problem of many poorly soluble drugs, has recently demonstrated [...] Read more.
The low solubility and bioavailability of aqueous insoluble drugs are critical challenges in the field of pharmaceuticals that need to be overcome. Nanocrystal technology, a novel pharmacological route to address the poor aqueous solubility problem of many poorly soluble drugs, has recently demonstrated great potential for industrial applications and developments. This review focuses on today’s preparation technologies, containing top-down, bottom-up, and combinative technology. Among them, the highlighted combinative technology can improve the efficiency of particle size reduction and overcome the shortcomings of a single technology. Then, the characterization methods of nanocrystal production are presented in terms of particle size, morphology, structural state, and surface property. After that, we introduced performance evaluations on the stability, safety, and the in vitro/in vivo dissolution of drug nanocrystals. Finally, the applications and prospects of nanocrystals in drug development are presented. This review may provide some references for the further development and optimization of poorly soluble drug nanocrystals. Full article
(This article belongs to the Special Issue Crystallization Process and Simulation Calculation)
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