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Journal articles on the topic 'Solid state polymorphic transformations'

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Author: Grafiati

Published: 10 December 2022

Last updated: 28 January 2023

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1

Hansen, Steve C., and D. Kobertz. "Solid-State Transformations in Metal Iodides." Solid State Phenomena 138 (March 2008): 29–42. http://dx.doi.org/10.4028/www.scientific.net/ssp.138.29.

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Numerous solid-state transformations occur in metal iodides. These transformations can be classified into three categories: polymorphic transformations, polytypic transitions and molecular solids. Many of the modifications of metal iodides involve metastable phases transforming into stable phases. Revisions to the In-I and Th-I phase diagrams are made based on data found in the literature.

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2

Tschauner, Oliver. "Corresponding States for Volumes of Elemental Solids at Their Pressures of Polymorphic Transformations." Crystals 12, no. 12 (November 23, 2022): 1698. http://dx.doi.org/10.3390/cryst12121698.

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Many non-molecular elemental solids exhibit common features in their structures over the range of 0 to 0.5 TPa that have been correlated with equivalent valence electron configurations. Here, it is shown that the pressures and volumes at polymorphic transitions obey corresponding states given by a single, empirical universal step-function Vtr/L = −0.0208(3) · Ptr + Ni, where Vtr is the atomic volume in Å3 at a given transformation pressure Ptr in GPa, and L is the principal quantum number. Ni assumes discrete values of approximately 20, 30, 40, etc. times the cube of the Bohr radius, thus separating all 113 examined polymorphic elements into five discrete sets. The separation into these sets is not along L. Instead, strongly contractive polymorphic transformations of a given elemental solid involve changes to different sets. The rule of corresponding states allows for predicting atomic volumes of elemental polymorphs of hitherto unknown structures and the transitions from molecular into non-molecular phases such as for hydrogen. Though not an equation of state, this relation establishes a basic principle ruling over a vast range of simple and complex solid structures that confirms that effective single-electron-based calculations are good approximations for these materials and pressures The relation between transformation pressures and volumes paves the way to a quantitative assessment of the state of very dense matter intermediate between the terrestrial pressure regime and stellar matter.

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3

Maher, Anthony, Colin C. Seaton, Sarah Hudson, Denise M. Croker, Åke C. Rasmuson, and Benjamin K. Hodnett. "Investigation of the Solid-State Polymorphic Transformations of Piracetam." Crystal Growth & Design 12, no. 12 (November 15, 2012): 6223–33. http://dx.doi.org/10.1021/cg301418c.

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4

Kubicki, Maciej. "Structural Aspects of Phase Transitions." Solid State Phenomena 112 (May 2006): 1–20. http://dx.doi.org/10.4028/www.scientific.net/ssp.112.1.

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There are two kinds of structural transformations in the crystalline solid state: solid state reactions, in which the product chemically different from the starting material can be isolated, and polymorphic transitions, when the phases have different organization of identical molecules in the crystal structures. As a consequence, the starting and the final phases of a solid state reaction differ in the melt and vapor, while different polymorphic modifications are identical in melt or gas phase. Some examples of the different phase transitions in the solid state are described in detail: the π-molecular complexes, the hydrogen-bond transformations and the reversible single crystal - twin transition.

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5

Einhorn, Cathy, André Durif, Marie-Thérèse Averbuch, and Jacques Einhorn. "Solid-State Isomerization of Atropodiastereomers: Effective Diastereoselection through Polymorphic Transformations." Angewandte Chemie 113, no. 10 (May 18, 2001): 1980–83. http://dx.doi.org/10.1002/1521-3757(20010518)113:10<1980::aid-ange1980>3.0.co;2-t.

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6

Einhorn, Cathy, André Durif, Marie-Thérèse Averbuch, and Jacques Einhorn. "Solid-State Isomerization of Atropodiastereomers: Effective Diastereoselection through Polymorphic Transformations." Angewandte Chemie International Edition 40, no. 10 (May 18, 2001): 1926–29. http://dx.doi.org/10.1002/1521-3773(20010518)40:10<1926::aid-anie1926>3.0.co;2-3.

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7

Makudera, A. O., and S. M. Lakiza. "Interaction in the systems Y2O3−Ln2O3 (Ln=Tb–Lu)." Uspihi materialoznavstva 2021, no. 2 (June 1, 2021): 72–78. http://dx.doi.org/10.15407/materials2021.02.072.

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Based on the analysis of literature data from experimentally constructed phase diagrams of Y2O3 − Ln2O3 systems (Ln = Tb − Lu), as well as temperatures of polymorphic transformations of rare earth oxides (REE), tentative phase diagrams of Y2O3 − Ln2O3 systems (Ln = Tb − Lu) were constructed in wide intervals of temperatures and concentrations. Prediction of the binary phase diagrams structure of yttria − yttrium subgroup lanthanides systems was carried out on the basis of three principles: 1. Since double systems are formed by lanthanide oxides of one (yttrium) subgroup, it is very likely that in such systems continuous solid solutions will be formed between the components. 2. Intermediate binary phases are not formed in these systems. 3. The formation of continuous solid solutions occurs with a decrease in the temperatures of phase transformations in the solid state to a minimum shifted towards a lower transformation temperature of the system component. The forecast of the Y2O3 – Ln2O3 systems phase diagrams structure, where Ln = Tb – Lu, indicates the complete solubility of the components in the liquid and solid states. Binary compounds in the considered systems are not predicted. Phase transformations in the solid solutions on the basis of polymorphic modifications X, H, A, B and C of lanthanide oxides cascade at high temperatures by the peritectoid mechanism. Below 1850 °C regions of solid solutions with cubic C-structure of REE oxides are formed in the whole range of concentrations in the systems. Key words: REE oxides, yttria, polymorphs of REE oxides, phase diagram.

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8

Tian, Beiqian, Zhiyong Ding, Shuyi Zong, Jinyue Yang, Na Wang, Ting Wang, Xin Huang, and Hongxun Hao. "Manipulation of Pharmaceutical Polymorphic Transformation Process Using Excipients." Current Pharmaceutical Design 26, no. 21 (June 24, 2020): 2553–63. http://dx.doi.org/10.2174/1381612826666200213122302.

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Background: In the pharmaceutical field, it is vital to ensure a consistent product containing a single solid-state form of the active pharmaceutical ingredient (API) in the drug product. However, some APIs are suffering from the risk of transformation of their target forms during processing, formulation and storage. Methods: The purpose of this review is to summarize the relevant category of excipients and demonstrate the availability and importance of using excipients as a key strategy to manipulate pharmaceutical polymorphic transformation. Results: The excipient effects on solvent-mediated phase transformations, solid-state transitions and amorphous crystallization are significant. Common pharmaceutical excipients including amino acids and derivatives, surfactants, and various polymers and their different manipulation effects were summarized and discussed. Conclusion: Appropriate use of excipients plays a role in manipulating polymorphic transformation process of corresponding APIs, with a promising application of guaranteeing the stability and effectiveness of drug dosage forms.

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9

Hsu, Cheng-Hung, Wen-Ting Ke, and Shan-Yang Lin. "Progressive Steps of Polymorphic Transformation of Gabapentin Polymorphs Studied by Hot-stage FTIR Microspectroscopy." Journal of Pharmacy & Pharmaceutical Sciences 13, no. 1 (April 8, 2010): 67. http://dx.doi.org/10.18433/j3fs32.

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Purpose. The aim of this study was to determine the progressive processes of polymorphic transformation of different gabapentin (GBP) polymorphs by using hot-stage Fourier transform infrared (FTIR) microspectroscopy. Methods. Four polymorphs of GBP were previously prepared and then identified by differential scanning calorimetry (DSC), thermogravimetric (TG) analysis, FTIR microspectroscopy and X-ray powder diffractometry. A novel hot-stage FTIR microspectroscopic technique was used to investigate the progressive steps of polymorphic transformation of each GBP polymorph sealed within two pieces of KBr plates. Results. Four polymorphs (Forms I, II, III and IV) of GBP were well characterized. The GBP form I was proven to be a monohydrate, but other GBP forms II-IV were anhydrous. Different thermal-induced progressive processes and steps of polymorphic interconversion of GBP polymorphs were clearly found from the changes in the three-dimensional IR spectral contour and peak intensity by using hot-stage FTIR microspectroscopy. The results also indicate that GBP form I was dehydrated and transformed to form III, and then converted to form IV; whereas GBP forms II and III directly transformed to form IV during heating. The GBP form IV was the last polymorph before the intramolecular lactamization of GBP. Conclusion. A one-step novel hot-stage FTIR microspectroscopy was successfully applied to simultaneously and continuously investigate the progressive processes and steps of thermal-induced polymorphic interconversion of GBP polymorph in the solid state.

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10

Wright, James S., Iñigo J. Vitórica-Yrezábal, Harry Adams, Stephen P. Thompson, Adrian H. Hill, and Lee Brammer. "Solvent-vapour-assisted pathways and the role of pre-organization in solid-state transformations of coordination polymers." IUCrJ 2, no. 2 (February 26, 2015): 188–97. http://dx.doi.org/10.1107/s2052252515000147.

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A family of one-dimensional coordination polymers, [Ag4(O2C(CF2)2CF3)4(phenazine)2(arene)n]·m(arene),1(arene = toluene or xylene), have been synthesized and crystallographically characterized. Arene guest loss invokes structural transformations to yield a pair of polymorphic coordination polymers [Ag4(O2C(CF2)2CF3)4(phenazine)2],2aand/or2b, with one- and two-dimensional architectures, respectively. The role of pre-organization of the polymer chains of1in the selectivity for formation of either polymorph is explored, and the templating effect of toluene andp-xylene overo-xylene orm-xylene in the formation of arene-containing architecture1is also demonstrated. The formation of arene-free phase2b, not accessible in a phase-pure form through other means, is shown to be the sole product of loss of toluene from1-tol·tol[Ag4(O2C(CF2)2CF3)4(phenazine)2(toluene)]·2(toluene), a phase containing toluene coordinated to Ag(I) in an unusual μ:η1,η1manner. Solvent-vapour-assisted conversion between the polymorphic coordination polymers and solvent-vapour influence on the conversion of coordination polymers1to2aand2bis also explored. The transformations have been examined and confirmed by X-ray diffraction, NMR spectroscopy and thermal analyses, includingin situdiffraction studies of some transformations.

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11

Dzyabchenko, A. "Prediction of polymorphic structures and solid state transformations of organic crystals." Acta Crystallographica Section A Foundations of Crystallography 58, s1 (August 6, 2002): c195. http://dx.doi.org/10.1107/s0108767302092802.

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12

Batisai, Eustina, Vincent J. Smith, Susan A. Bourne, and Nikoletta B. Báthori. "Solid state structures ofp-cresol revisited." CrystEngComm 17, no. 28 (2015): 5134–38. http://dx.doi.org/10.1039/c4ce02334j.

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13

Nyström, Maija, Jorma Roine, Matti Murtomaa, R. Mohan Sankaran, Hélder A. Santos, and Jarno Salonen. "Solid state transformations in consequence of electrospraying – A novel polymorphic form of piroxicam." European Journal of Pharmaceutics and Biopharmaceutics 89 (January 2015): 182–89. http://dx.doi.org/10.1016/j.ejpb.2014.11.027.

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14

An, Ji-Hun, Wonno Youn, Alice Kiyonga, Changjin Lim, Minho Park, Young-Ger Suh, Hyung Ryu, Jae Kim, Chun-Woong Park, and Kiwon Jung. "Kinetics of the Solution-Mediated Polymorphic Transformation of the Novel l-Carnitine Orotate Polymorph, Form-II." Pharmaceutics 10, no. 4 (October 1, 2018): 171. http://dx.doi.org/10.3390/pharmaceutics10040171.

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Research studies related to the polymorphs of l-Carnitine orotate (CO), a medication used for the treatment and prevention of liver diseases, are insignificant or almost nonexistent. Accordingly, in the present study, l-Carnitine orotate (CO) was prepared for investigating CO polymorphs. Here, a reactive crystallization was induced by reacting 1g of l-Carn (1 equivalent) and 0.97 g of OA (1 equivalent) in methanol (MeOH); as a result, CO form-I and CO form-II polymorphs were obtained after 1 h and 16 h of stirring, respectively. The characterization of CO polymorphs was carried out utilizing Powder X-ray diffraction (PXRD), Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA) and solid-state Nuclear Magnetic Resonance Spectroscopy (solid-state CP/MAS 13C-NMR). The solution-mediated polymorphic transformation (SMPT) of CO polymorphs was investigated in MeOH at controlled temperature and fixed rotational speed. The results revealed that CO form-I is a metastable polymorph while CO form-II is a stable polymorph. From the same results, it was confirmed that CO form-I was converted to CO form-II during the polymorphic phase transformation process. Moreover, it was assessed that the increase in temperature and supersaturation level significantly promotes the rate of nucleation, as well as the rate of mass transfer of CO form-II. In addition, nucleation and mass transfer equations were employed for the quantitative determination of SMPT experimental results. Lastly, it was suggested that CO form-II was more thermodynamically stable than CO form-I and that both polymorphs belong to the monotropic system.

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15

Jing, Dingding, Yuan Gu, and Huiming Xia. "Solid-State and Solution-Mediated Polymorphic Transformation of Rifampicin." Chemical Engineering & Technology 41, no. 6 (May 3, 2018): 1236–43. http://dx.doi.org/10.1002/ceat.201700233.

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16

Bulutoglu, Pelin Su, Conor Parks, Nandkishor K. Nere, Shailendra Bordawekar, and Doraiswami Ramkrishna. "Exploring New Crystal Structures of Glycine via Electric Field-Induced Structural Transformations with Molecular Dynamics Simulations." Processes 7, no. 5 (May 8, 2019): 268. http://dx.doi.org/10.3390/pr7050268.

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Being able to control polymorphism of a crystal is of great importance to many industries, including the pharmaceutical industry, since the crystal’s structure determines significant physical properties of a material. While there are many conventional methods used to control the final crystal structure that comes out of a crystallization unit, these methods fail to go beyond a few known structures that are kinetically accessible. Recent studies have shown that externally applied fields have the potential to effectively control polymorphism and to extend the set of observable polymorphs that are not accessible through conventional methods. This computational study focuses on the application of high-intensity dc electric fields (e-fields) to induce solid-state transformation of glycine crystals to obtain new polymorphs that have not been observed via experiments. Through molecular dynamics simulations of solid-state α -, β -, and γ -glycine crystals, it has been shown that the new polymorphs sustain their structures within 125 ns after the electric field has been turned off. It was also demonstrated that strength and direction of the electric field and the initial structure of the crystal are parameters that affect the resulting polymorph. Our results showed that application of high-intensity dc electric fields on solid-state crystals can be an effective crystal structure control method for the exploration of new crystal structures of known materials and to extend the range of physical properties a material can have.

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17

Bond, Andrew, Dhara Raijada, Jukka Rantanen, Ioana Sovago, Jacco van de Streek, Flemming Larsen, and Diana Thomas. "In situ monitoring of hydration and dehydration in pharmaceutical solids." Acta Crystallographica Section A Foundations and Advances 70, a1 (August 5, 2014): C906. http://dx.doi.org/10.1107/s2053273314090937.

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This talk will describe a multi-technique study of hydration and dehydration in pharmaceutical solids, using sodium naproxen as a case study. The aim of the work is to establish molecular-level structural understanding of the chemical changes that take place in the solid state as a function of temperature and relative humidity. Dynamic vapour sorption (DVS) analysis on the anhydrous compound carried out as a function of temperature provides a preliminary overview of the solid-form landscape and identifies static conditions to obtain four different hydrate forms [1]. Differences in the sorption and desorption cycles indicates the existence of a polymorphic dihydrate, and the two polymorphs show significant differences in their dehydration behaviour. Crystal structures are established for all phases in the system using either single-crystal or powder X-ray diffraction data, supplemented by dispersion-corrected density functional theory (DFT-D) calculations. The hydration and dehydration processes are monitored by powder X-ray diffraction (PXRD), as a function of relative humidity and temperature, and by variable-temperature solid-state 13C and 23Na NMR. Synchrotron PXRD is applied to the two dihydrate polymorphs to monitor the dehydration processes in approximately real time. The kinetic and structural details of dehydration are established by applying parametric Rietveld refinement [2] to the synchrotron data. This approach adds a structural picture to the kinetic processes. The PXRD studies indicate an essentially continuous dehydration pathway from one of the dihydrate polymorphs to the monohydrate, but a stepped dehydration pathway for the other dihydrate polymorph. The different mechanisms are linked to different degrees of structural similarity, and in particular to the existence of topotactic or non-topotactic transformations between the dihydrate polymorphs and the unique monohydrate and anhydrate phases.

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18

Shi, Genpei, Si Li, Peng Shi, Junbo Gong, Mingtao Zhang, and Weiwei Tang. "Distinct pathways of solid-to-solid phase transitions induced by defects: the case of DL-methionine." IUCrJ 8, no. 4 (May 8, 2021): 584–94. http://dx.doi.org/10.1107/s2052252521004401.

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Understanding of solid-to-solid phase transition mechanisms in polymorphic systems is of critical importance for rigorous control over polymorph purity in the pharmaceutical industry to achieve the desired bioavailability and efficacy of drugs. Ubiquitous defects in crystals may play an important role in the pathways of phase transitions. However, such effects remain poorly understood. Here, the effects of crystal defects on the solid-to-solid phase transformations between DL-methionine polymorphs α and β are investigated by means of experimental and computational approaches. Thermal analyses of polycrystalline powders show two endothermic peaks in the α-to-β phase transition (and two exothermic peaks for the reverse transition), in contrast with one thermal event observed for single crystals. Variable-temperature 1D and 2D Raman spectra, as well as powder X-ray diffraction patterns, reveal the appearance of two peaks that can attributed to a two-step phase transition, and the extent of the second-step phase transition increases with milling time (or defect density). Quantification of transition kinetics unveils a remarkably higher energy barrier in the second-step phase transition than in the first, proceeding by the cooperative molecular motion pathway. The good linear fitting on the kinetic data by the Jeziorny model suggests that the second-step transition follows the nucleation and growth mechanism. Molecular dynamics simulations were also conducted to understand the role of crystal defects in the solid-state phase transition by tracking the atomic distribution and hydrogen bond lifetime during the transition. It was found that the increasing defect density hinders the propagation of cooperative molecular motion, leading to a combined transition mechanism involving both cooperative motion and nucleation and growth. This study highlights the significant impact of crystal defects on solid-state phase transitions, and the two-step transition mechanism postulated may be universal given the ubiquitous presence of defects in crystalline materials.

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19

Shen, Xiaoqin, Yonghao Zheng, and Fred Wudl. "Thermally induced reversible solid-state transformation of novel s-indacene 1,3,5,7-tetraone derivatives." Journal of Materials Chemistry C 4, no. 13 (2016): 2427–31. http://dx.doi.org/10.1039/c5tc03953c.

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20

Araya-Sibaja, Andrea Mariela, Amarilis Scremin Paulino, Gabriela Schneider Rauber, Carlos Eduardo Maduro Campos, Simone Gonçalves Cardoso, Gustavo Alberto Monti, Valeria Heredia, Ismael Bianco, Dante Beltrano, and Silvia Lucia Cuffini. "Dissolution properties, solid-state transformation and polymorphic crystallization: progesterone case study." Pharmaceutical Development and Technology 19, no. 7 (September 13, 2013): 779–88. http://dx.doi.org/10.3109/10837450.2013.829096.

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21

Ruggiero, Michael T., J. Axel Zeitler, and Timothy M. Korter. "Concomitant polymorphism and the martensitic-like transformation of an organic crystal." Physical Chemistry Chemical Physics 19, no. 42 (2017): 28502–6. http://dx.doi.org/10.1039/c7cp04666a.

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22

Campos, Joana R., Ana R. Fernandes, Patricia Severino, Maria L. Gracia, Selma B. Souto, and Eliana B. Souto. "Phase Behavior of Polymorphic Fats in Drug Delivery Systems - A Review of the State of Art." Current Pharmaceutical Design 24, no. 21 (October 15, 2018): 2508–12. http://dx.doi.org/10.2174/1381612824666180522092740.

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Fats are essential nutrients that have a significant role in the human diet and are essential to provide energy. Fatty acids are present in several types of lipids, such as triglycerides and phospholipids. Fatty acids differ among them, depending on the number of double bonds and on the length of the hydrocarbon chains. If there are no double bonds, the fatty acids are considered saturated and show a linear structure. Compounds with double bonds are unsaturated and have bent structure. The saturated fatty acids are usually solid at room temperature and the unsaturated fatty acids are liquid at that very same temperature. These compounds are of recognized value as raw materials for drug delivery systems, such as lipid nanoparticles. The behaviour of the macroscopic aspects of fat polymorphisms is directly influenced by the melting point, the crystallization and their polymorphic transformations. In this work, we revise the most critical factors contributing for the long-term stability of lipid nanoparticles, as well as the influence of the polymorphism on the loading capacity for drug molecules.

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23

Donia, Ahmed M., Saëda Abou El-Enein, and Mamdouh S. Masoud. "Solid-state thermal polymorphic transformations for some solvates of 2-hydroxy-5-methylazobenzene-4'-carboxylic acid complexes." Thermochimica Acta 161, no. 2 (May 1990): 217–22. http://dx.doi.org/10.1016/0040-6031(90)80303-g.

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24

Pan, Bochen, Leping Dang, Zhanzhong Wang, Jun Jiang, and Hongyuan Wei. "Preparation, crystal structure and solution-mediated phase transformation of a novel solid-state form of CL-20." CrystEngComm 20, no. 11 (2018): 1553–63. http://dx.doi.org/10.1039/c7ce02026k.

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25

OTSUKA, MAKOTO, TAKAHIRO MATSUMOTO, and NOBUYOSHI KANENIWA. "Effect of environmental temperature on polymorphic solid-state transformation of indomethacin during grinding." CHEMICAL & PHARMACEUTICAL BULLETIN 34, no. 4 (1986): 1784–93. http://dx.doi.org/10.1248/cpb.34.1784.

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26

Krivchikov, Alexander, Ove Andersson, Oksana Korolyuk, and Oleksii Kryvchikov. "Thermal Conductivity of Solid Triphenyl Phosphite." Molecules 27, no. 23 (December 1, 2022): 8399. http://dx.doi.org/10.3390/molecules27238399.

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The thermal conductivity, κ, of solid triphenyl phosphite was measured by using the transient hot-wire method, and its temperature and pressure dependencies were analyzed to understand heat transfer processes in the solid polymorphic phases, as well as in the glass and the exotic glacial state. Phase transformations and the structural order of the phases are discussed, and a transitional pressure–temperature diagram of triphenyl phosphite is presented. The thermal conductivity of both the crystalline and disordered states is described within the theory of two-channel heat transfer by phonons and diffusons in dielectric solids. In the glass and glacial states, the weakly temperature-dependent (glass-like) κ is described well by the term associated with heat conduction of diffusons only, and it can be represented by an Arrhenius-type function. In the crystal phases, the strongly temperature-dependent (crystal-like) κ associated with heat transfer by phonons is weakened by significant heat transfer by diffusons, and the extent of the two contributions is reflected in the temperature dependence of κ. We find that the contribution of diffusons in the crystal phases depends on pressure in the same way as that in amorphous states, thus indicating that the same mechanism is responsible for this channel of heat transfer in crystals and amorphous states.

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27

Bayard, F., C. Decoret, and J. Royer. "The Atom-Atom Potential Method as an Aid in Determining Possible Pathways of Polymorphic Transformations in the Solid State." Molecular Crystals and Liquid Crystals 156, no. 1 (March 1, 1988): 185–91. http://dx.doi.org/10.1080/00268948808070567.

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28

Bayard, F., C. Decoret, and J. Royer. "The Atom-Atom Potential Method as an Aid in Determining Possible Pathways of Polymorphic Transformations in the Solid State." Molecular Crystals and Liquid Crystals Incorporating Nonlinear Optics 156, no. 1 (March 1988): 185–91. http://dx.doi.org/10.1080/10441859.1988.11009195.

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29

Dametto, P. R., A. B. Siqueira, C. T. Carvalho, and M. Ionashiro. "Synthesis, characterization and thermal studies on solid state 3-methoxybenzoate of lighter trivalent lanthanides." Eclética Química 32, no. 2 (2007): 17–21. http://dx.doi.org/10.1590/s0100-46702007000200003.

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Solid-state Ln -3-MeO-Bz compounds, where Ln stands for lighter trivalent lanthanides (La Sm) and 3-methoxybenzoate, have been synthesized. Thermogravimetry (TG), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy, and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information concerning the composition, dehydration, polymorphic transformation, thermal behaviour and thermal decomposition of the synthesized compounds.

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30

Lin, Shan-Yang. "An Overview of Famotidine Polymorphs: Solid-State Characteristics, Thermodynamics, Polymorphic Transformation and Quality Control." Pharmaceutical Research 31, no. 7 (March 1, 2014): 1619–31. http://dx.doi.org/10.1007/s11095-014-1323-5.

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31

Somidin, Flora, Hiroshi Maeno, Xuan Tran, Stuart D. McDonald, Mohd Mohd Salleh, Syo Matsumura, and Kazuhiro Nogita. "Imaging the Polymorphic Transformation in a Single Cu6Sn5 Grain in a Solder Joint." Materials 11, no. 11 (November 9, 2018): 2229. http://dx.doi.org/10.3390/ma11112229.

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In-situ observations of the polymorphic transformation in a single targeted Cu6Sn5 grain constrained between Sn-0.7 wt % Cu solder and Cu-Cu3Sn phases and the associated structural evolution during a solid-state thermal cycle were achieved via a high-voltage transmission electron microscope (HV-TEM) technique. Here, we show that the monoclinic η′-Cu6Sn5 superlattice reflections appear in the hexagonal η-Cu6Sn5 diffraction pattern upon cooling to isothermal 140 °C from 210 °C. The in-situ real space imaging shows that the η′-Cu6Sn5 contrast pattern is initiated at the grain boundary. This method demonstrates a new approach for further understanding the polymorphic transformation behavior on a real solder joint.

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32

Croitor, Lilia, Mihaela F. Petric, Elisabeta I. Szerb, Gabriela Vlase, Paulina N. Bourosh, Yurii M. Chumakov, and Manuela E. Crisan. "The role of 4-nitrobenzoic acid polymorphs in the crystallization process of organic acid–base multicomponent systems." CrystEngComm 21, no. 40 (2019): 6038–47. http://dx.doi.org/10.1039/c9ce01239g.

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An investigation of the role of 4-nitrobenzoic acid polymorphs in the crystallization process of dimethylethanolammonium 4-nitrobenzoate from solution and comprehensive characterization of time-dependent changes associated with solid-state transformations are presented.

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33

Goloveshkin, Alexander S., Alexander A. Korlyukov, and Anna V. Vologzhanina. "Novel Polymorph of Favipiravir—An Antiviral Medication." Pharmaceutics 13, no. 2 (January 21, 2021): 139. http://dx.doi.org/10.3390/pharmaceutics13020139.

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Various solid forms of pharmaceutically important compounds exhibit different physical properties and bioactivity; thus, knowledge of the structural landscape and prediction of spontaneous polymorph transformations for an active pharmaceutical ingredient is of practical value for the pharmaceutical industry. By recrystallization from ethyl acetate, a novel polymorph of 6-fluoro-3-hydroxypyrazine-2-carboxamide (trademark favipiravir, RNA polymerase inhibitor) was obtained and characterized using differential scanning calorimetry (DSC), infra-red spectroscopy and powder X-ray diffraction (XRD) analysis. The favipiravir molecule in two polymorphs realizes similar H-bonding motifs, but the overall H-bonded networks differ. Based on periodic density functional theory calculations, the novel tetragonal polymorph with two interpenetrated H-bonded networks is slightly less stable than the orthorhombic one with the zst topology of the underlying H-bonded net that is in accord with experimentally observed powder XRD patterns of slow conversion of the tetragonal phase to the orthorhombic one. However, topological analysis of net relations revealed that no transformations can be applied to convert H-bonded networks in the experimental unit cells, and DSC data indicate no solid-state reactions at heating.

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34

Yamanobe, Maiko, Hiroshi Takiyama, and Masakuni Matsuoka. "Kinetic Study on Polymorphic Solid-State Transformation of Organic Compounds: Bisphenol A and DL-Methionine." JOURNAL OF CHEMICAL ENGINEERING OF JAPAN 35, no. 3 (2002): 247–54. http://dx.doi.org/10.1252/jcej.35.247.

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35

da Silva, Lucélia, Cristina Montanari, Marilene Ângelo, Edith Cristina Cazedey, Rudy Bonfilio, and Magali Araújo. "Evaluation of Polymorphism Influence in the Finasteride." Acta Crystallographica Section A Foundations and Advances 70, a1 (August 5, 2014): C1567. http://dx.doi.org/10.1107/s2053273314084320.

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Finasteride is a specific competitive inhibitor of steroid type-II 5α-reductase, an intracellular enzyme that converts testosterone to dihydrotestosterone (DHT) and is widely used for the treatment of benign prostatic hyperplasia (BPH), prostate cancer , and androgenetic alopecia. Polymorphs are known to give rise to significant differences in the physicochemical properties of the compound as melting point, density, morphology, solubility and colour. Thus, proper monitoring of solid-state forms, both qualitative and quantitative, is crucial in order to ensure high-quality products. The crystal structures of finasteride appear in the Cambridge Crystal Structure Database (CSD) under the codes WOLXOK01 and WOLXOK02 for Form I and WOLXOK03 for Form II. In this context, the aim of this work was study the behavior of the chemical structure and physicochemical properties of polymorphic forms, and to evaluate the possible influence in the dissolution profile and stability of capsules. A stability study was carried out at 500C for 3 months. The Form II of finasteride was obtained by heating Form I to 2350C for 30 minutes. The techniques X-ray diffraction, infrared spectroscopy and thermal analysis were applied to characterize the Forms. The solubility of finasteride polymorphs was determined by equilibrium solubility method. For the dissolution test, water was used as dissolution medium and the basket apparatus at 100 rpm. The samples were analyzed by HPLC at 210 nm. Differences in X-ray diffraction and infrared spectra of the two polymorphs were observed. The DSC curves showed Form I melting peak at 2570C and solid-solid transformation to Form II at about 2300C. In the solubility study was observed higher Form II solubility than Form I in most evaluated pHs. The interaction of the Forms I and II with capsule excipients may have been different since the dissolution profile of the capsules showed higher release to the Form I. In the stability study, the finasteride content was stable for two Forms, however, the dissolution profile of Form II showed greater decline than the Form I. In conclusion, the results show that the dissolution profiles polymorphism may influence the quality of finasteride capsules, being necessary there be a polymorphic quality control for this dosage Form. Acknowledgments: PNPD CAPES and FAPEMIG

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Halasz, Ivan, Mirta Rubčić, Krunoslav Užarević, Ivica Đilović, and Ernest Meštrović. "The cocrystal of 4-oxopimelic acid and 4,4′-bipyridine: polymorphism and solid-state transformations." New J. Chem. 35, no. 1 (2011): 24–27. http://dx.doi.org/10.1039/c0nj00569j.

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37

Rodrigues, E. C., A. B. Siqueira, E. Y. Ionashiro, G. Bannach, and M. Ionashiro. "Synthesis, characterization and thermal behaviour of solid-state compounds of 4-methoxybenzoate with lanthanum (III) and trivalent lighter lanthanides." Eclética Química 31, no. 1 (2006): 21–30. http://dx.doi.org/10.1590/s0100-46702006000100003.

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Solid-state M-4-MeO-Bz compounds, where M stands for trivalent La, Ce, Pr, Nd and Sm and 4-MeO-Bz is 4-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, polymorphic transformation, ligand's denticity, thermal behaviour and thermal decomposition of the isolated compounds.

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Kumar, Sujeet, S. J. Burns, and T. N. Blanton. "Growth kinetics, phase transitions, and cracking in cholesterol gallstones." Journal of Materials Research 10, no. 1 (January 1995): 216–24. http://dx.doi.org/10.1557/jmr.1995.0216.

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The growth kinetics of cholesterol gallstones have been studied by growing crystals from melted gallstones. The resulting microstructures are spherulitic which is essentially the same as the structures seen in natural gallstones prior to melting. The cholesterol crystals when observed in hot stage microscopy emerge from a unique nucleation center growing radially in the [001] direction with constant rate. The DSC thermograph of a natural gallstone is initially similar to that of cholesterol monohydrate. Upon melting, cholesterol monohydrate changes to anhydrous cholesterol; both forms are crystalline and exhibit polymorphic transformations. Synthetic stones grown from cholesterol were anhydrous and have a phase change at temperatures close to human body temperature. Optical microscopy established that this phase transformation cracks the spherulitic crystals perpendicular to the fast growth direction. Thermal expansion measurements demonstrate that upon heating, the low density, low temperature phase is transformed to a high density phase. This phase transformation and repeated cracking may prove to be useful in destroying natural gallstones, while suppressing this transformation and its associated cracking might aid in securing other solid cholesterol deposits within the human body.

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Trush, Vasyl, Alexander Luk’yanenko, and Viktor Fedirko. "Study of titanium oxidation kinetics at temperature above polymorphic transformation." Technology audit and production reserves 4, no. 1(60) (July 27, 2021): 37–41. http://dx.doi.org/10.15587/2706-5448.2021.237250.

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The object of research is the analytical description of the phenomena in the near-surface layer, which are caused by the interaction of titanium with oxygen at high temperatures. These are temperatures that exceed the polymorphic transformation of the metal. High-temperature oxidation gives titanium products unique performance properties. Of course, such characteristics are determined, first of all, by the state of the near-surface layer. Therefore, an understanding of oxidation processes will make it possible to predict the state of the near-surface layer after heat treatment. However, to date, no unified approach has been created to describe the mechanism and kinetics of high-temperature oxidation of titanium in the near-surface layer. Indeed, most of the existing approaches make it possible to predict the nature of oxidation in the bulk of the metal. Some scientific papers describe the kinetics of oxidation, taking into account only the formation and growth of oxide layers. However, simultaneously with oxide formation, a diffusion zone is formed, which significantly affects the kinetics. Therefore, today one of the most problematic areas of high-temperature titanium oxidation is the description of the processes that take place in the near-surface layer. In this work, to describe the kinetics of high-temperature oxidation of titanium, in addition to the formation and growth of the oxide layer, the formation and growth of the diffusion zone is taken into account. In the diffusion zone, under the influence of structural phase transformations, solid solutions of oxygen are formed in the alpha and beta phases. This approach made it possible to take into account additional factors and thereby more accurately describe the processes of high-temperature oxidation of titanium. As a result of the calculations, the thickness of the oxide layer of the diffusion zone is given depending on the oxygen concentration and the duration of treatment. And also the dependences of the kinetics of displacement of the boundary of the oxide-diffusion layer are given and a system of equations for calculating the ratio of the formed phase components is developed. Thanks to the proposed analytical approach, it will be possible to calculate the sizes of interphase boundaries on the basis of temperature-time parameters and oxygen concentration and thereby form a hardened near-surface layer with certain functional properties

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O'Mahony, Marcus, Anthony Maher, Denise Croker, Ake Rasmuson, and Benjamin Hodnett. "Redefining Solution-Mediated Transformations: Pharmaceutical Systems." Acta Crystallographica Section A Foundations and Advances 70, a1 (August 5, 2014): C1571. http://dx.doi.org/10.1107/s2053273314084289.

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Engineering the isolation of a metastable or stable crystalline phase of an active pharmaceutical ingredient (API) is of critical importance when crystallizing from solution as an uncontrolled outcome can directly affect API manufacture and performance. The theoretical framework for understanding solution-mediated crystal phase or polymorphic transformation (SMPT) was first established by Cardew & Davey.[1] The process is defined to consist of a metastable phase that dissolves and a stable phase that nucleates and grows independently from the solution. That paper also identified that in terms of a reaction pathway, SMPT could be controlled in either of two ways: by growth of the stable phase or dissolution the metastable phase. Studies concerning SMPT since then have brought the definition and those conclusions into question. Firstly, the recent case of the SMPT from FI to FIII carbamazepine and FII to FIII piractem were studied separately where data on both the solid state composition and solution concentration were collected during the transformation using powder X-ray diffraction and in situ infra-red spectroscopy, respectively. These studies, in combination with a brief review of the literature, reveal that SMPT can be controlled not only in the two ways described by Cardew & Davey but rather in 4 principal ways (Figure 1).[2] Secondly, many studies now identify that nucleation of the stable phase often occurs on the surface of the metastable phase during SMPT [3] and not independently from solution. Again when the literature is examined, this surface supported nucleation event is identified as being either epitaxial in nature or having no or inconclusive evidence of epitaxy. It is concluded that the term "independently" in the definition by Cardew & Davey be redefined to recognize that the crystallization of the stable phase during SMPT is often dependent on the surface of the metastable phase in solution.

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O’Mahony, Marcus A., Anthony Maher, Denise M. Croker, Åke C. Rasmuson, and Benjamin K. Hodnett. "Examining Solution and Solid State Composition for the Solution-Mediated Polymorphic Transformation of Carbamazepine and Piracetam." Crystal Growth & Design 12, no. 4 (March 15, 2012): 1925–32. http://dx.doi.org/10.1021/cg201665z.

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Lust, Andres, Satu Lakio, Julia Vintsevits, Jekaterina Kozlova, Peep Veski, Jyrki Heinämäki, and Karin Kogermann. "Water-mediated solid-state transformation of a polymorphic drug during aqueous-based drug-layer coating of pellets." International Journal of Pharmaceutics 456, no. 1 (November 2013): 41–48. http://dx.doi.org/10.1016/j.ijpharm.2013.08.036.

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43

Sautel, M., G. Lépinasse, and F. Leveiller. "Study of the textural changes occurring during a solid state polymorphic transformation induced by temperature and relative humidity." Colloids and Surfaces A: Physicochemical and Engineering Aspects 187-188 (August 2001): 337–47. http://dx.doi.org/10.1016/s0927-7757(01)00649-5.

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44

Procházková, Eliška, Cheng Cao, Aditya Rawal, Martin Dračínský, Saroj Bhattacharyya, Ivana Císařová, James M. Hook, and Martina H. Stenzel. "Polymorphic Transformation of Drugs Induced by Glycopolymeric Vesicles Designed for Anticancer Therapy Probed by Solid-State NMR Spectroscopy." ACS Applied Materials & Interfaces 11, no. 31 (July 10, 2019): 28278–88. http://dx.doi.org/10.1021/acsami.9b05514.

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45

Ali, Hassan Refat H., Howell G. M. Edwards, and Ian J. Scowen. "Insight into thermally induced solid-state polymorphic transformation of sulfathiazole using simultaneousin situRaman spectroscopy and differential scanning calorimetry." Journal of Raman Spectroscopy 40, no. 8 (August 2009): 887–92. http://dx.doi.org/10.1002/jrs.2189.

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46

Zakirýanova, Irina D., Vladimir A. Khokhlov, Alexander B. Salyulev, and Iraida V. Korzun. "On Polymorphism of Dysprosium Trichloride." Zeitschrift für Naturforschung A 70, no. 3 (March 1, 2015): 153–57. http://dx.doi.org/10.1515/zna-2014-0276.

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AbstractFor the first time, the structure of crystalline DyCl3 over a wide temperature range from room temperature to melting point was studied by Raman spectroscopy. The phonon modes (cm–1) of dysprosium trichloride (monoclinic crystal lattice of AlCl3 type, Z=4, CN = 6) at room temperature are 257 (A1g), 201 (Eg), 112 (Eg), 88 (A1g), and 63 (Eg). The monoclinic structure of the crystalline DyCl3 C2h3 symmetry was found to remain constant over the studied temperature range. No polymorphic transformation in the solid state was detected. Gravimetry, calorimetry, and mass spectrometry have been used in addition to support the conclusions made on the basis of Raman spectroscopic data.

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Chaemchuen, Somboon, Kui Zhou, Mekhman S. Yusubov, Pavel S. Postnikov, Nikom Klomkliang, and Francis Verpoort. "Solid-state transformation in porous metal-organic frameworks based on polymorphic-pillared net structure: Generation of tubular shaped MOFs." Microporous and Mesoporous Materials 278 (April 2019): 99–104. http://dx.doi.org/10.1016/j.micromeso.2018.11.023.

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48

Shamshina, Julia L., and Robin D. Rogers. "Are Myths and Preconceptions Preventing Us from Applying Ionic Liquid Forms of Antiviral Medicines to the Current Health Crisis?" International Journal of Molecular Sciences 21, no. 17 (August 20, 2020): 6002. http://dx.doi.org/10.3390/ijms21176002.

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At the moment, there are no U.S. Food and Drug Administration (U.S. FDA)-approved drugs for the treatment of COVID-19, although several antiviral drugs are available for repurposing. Many of these drugs suffer from polymorphic transformations with changes in the drug’s safety and efficacy; many are poorly soluble, poorly bioavailable drugs. Current tools to reformulate antiviral APIs into safer and more bioavailable forms include pharmaceutical salts and cocrystals, even though it is difficult to classify solid forms into these regulatory-wise mutually exclusive categories. Pure liquid salt forms of APIs, ionic liquids that incorporate APIs into their structures (API-ILs) present all the advantages that salt forms provide from a pharmaceutical standpoint, without being subject to solid-state matter problems. In this perspective article, the myths and the most voiced concerns holding back implementation of API-ILs are examined, and two case studies of API-ILs antivirals (the amphoteric acyclovir and GSK2838232) are presented in detail, with a focus on drug property improvement. We advocate that the industry should consider the advantages of API-ILs which could be the genesis of disruptive innovation and believe that in order for the industry to grow and develop, the industry should be comfortable with a certain element of risk because progress often only comes from trying something different.

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49

Botoshansky, M., A. Ellern, N. Gasper, J. O. Henck, and F. H. Herbstein. "Structural, Thermodynamic and Kinetic (Hysteresis) Aspects of the Enantiotropic First-Order Phase Transformations of N-Anilinophthalimide and N-(N'-Methylanilino)phthalimide." Acta Crystallographica Section B Structural Science 54, no. 3 (June 1, 1998): 277–90. http://dx.doi.org/10.1107/s0108768197012135.

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The crystal structures of the orthorhombic and monoclinic polymorphs of N-anilinophthalimide (m.p. of monoclinic polymorph 457 K) have been determined by X-ray diffraction at 293 K and were found to have only small differences between the molecular conformations in the two phases, but quite different molecular arrangements. There is very weak N—H...O hydrogen bonding in the orthorhombic phase and weak N—H...O hydrogen bonding in the monoclinic phase. The thermal motion in the crystals of both phases has been analyzed and their thermal expansion determined. The enthalpies of solution in a number of solvents have been calculated from the solubility measurements of Chattaway & Lambert [(1915), J. Chem. Soc. 107, 1773–1781], which also give the temperature and enthalpy of the enantiotropic `orthorhombic to monoclinic' phase transformation (Tc = 283 K; ΔH transf = 1.54 kJ mol−1). The phase-transformation endotherm in a DSC (differential scanning calorimetry) trace from the orthorhombic polymorph occurs only at ∼310 K on heating and there is no corresponding exotherm on cooling; the DSC trace gives ΔH transf = 1.62 kJ mol−1 and ΔH fus = 26.9 kJ mol−1. This phase transformation is an example of the common type (occurrence ∼95%) where ΔV transf = (V monoclinic − V orthorhombic) is positive. Analogous (but less complete) results have been obtained for the monoclinic and triclinic polymorphs of N-(N′-methylanilino)phthalimide (m.p. of triclinic polymorph 398 K). There were only minor differences between the molecular conformations in the two phases, but the molecular arrangements were quite different. This `monoclinic to triclinic' phase transformation also has ΔV transf = (V triclinic − V monoclinic) positive. The solubility (and other) measurements of Chattaway & Lambert (1915) gave Tc = 328.43 K and ΔH transf = 4.17 kJ mol−1. A DSC trace for the monoclinic crystals shows a broad endotherm at ∼372–376 K on heating, but there is no corresponding exotherm on cooling; ΔH transf = 3.6 kJ mol−1 and ΔH fus = 21.7 kJ mol−1. These two compounds provide further examples of molecular crystals with a large hysteresis in their first-order enantiotropic solid-state phase transformations, the transformation to the high-temperature phase occurring well above Tc and the low-temperature phase not being recovered on cooling below Tc . Presumably the hysteresis must be ascribed to as-yet unknown features of the nucleation processes.

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Yu, Tong, Jiang Cheng, Lu Li, Benshuang Sun, Xujin Bao, and Hongtao Zhang. "Current understanding and applications of the cold sintering process." Frontiers of Chemical Science and Engineering 13, no. 4 (October 18, 2019): 654–64. http://dx.doi.org/10.1007/s11705-019-1832-1.

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Abstract In traditional ceramic processing techniques, high sintering temperature is necessary to achieve fully dense microstructures. But it can cause various problems including warpage, overfiring, element evaporation, and polymorphic transformation. To overcome these drawbacks, a novel processing technique called “cold sintering process (CSP)” has been explored by Randall et al. CSP enables densification of ceramics at ultra-low temperature (⩽300°C) with the assistance of transient aqueous solution and applied pressure. In CSP, the processing conditions including aqueous solution, pressure, temperature, and sintering duration play critical roles in the densification and properties of ceramics, which will be reviewed. The review will also include the applications of CSP in solid-state rechargeable batteries. Finally, the perspectives about CSP is proposed.

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