Temperature Behavior of Precursor Clusters at the Pre-Crystallization Phase of K(H<sub>2</sub>PO<sub>4</sub>) Studied by SAXS
Elementary building blocks for the growth of KDP crystals were established. The solution of potassium dihydrogen phosphate (KH2PO4–KDP) has been experimentally studied by the small-angle X-ray scattering (SAXS) method. The analysis of SAXS data in the temperature range of 2.5–90 °C using a set of mo...
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2022-12-01
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| author | Andrey E. Sukhanov Kseniia B. Ilina Petr V. Konarev Georgy S. Peters Yury V. Pisarevsky Ekaterina S. Smirnova Olga A. Alekseeva Mikhail V. Kovalchuk |
| author_facet | Andrey E. Sukhanov Kseniia B. Ilina Petr V. Konarev Georgy S. Peters Yury V. Pisarevsky Ekaterina S. Smirnova Olga A. Alekseeva Mikhail V. Kovalchuk |
| author_sort | Andrey E. Sukhanov |
| collection | DOAJ |
| description | Elementary building blocks for the growth of KDP crystals were established. The solution of potassium dihydrogen phosphate (KH2PO4–KDP) has been experimentally studied by the small-angle X-ray scattering (SAXS) method. The analysis of SAXS data in the temperature range of 2.5–90 °C using a set of models of 3D fragments of the crystal structure showed that the saturated solution contains above K<sup>+</sup>, H<sub>2</sub>PO<sub>4</sub><sup>−</sup> and KH<sub>2</sub>PO<sub>4</sub> monomers, as well as mainly octamers. The 3D model of the octamer isolated from the crystal structure has dimensions of 17.443 Å along the [001] axis and 5.963 Å along the [100] and [010] axes. As the temperature is decreased, starting from the saturation temperature of the solution, the volume fraction of octamers sharply increases while the volume fraction of monomers decreases. The results indicate that the monomers and octamers represent major components in the solution with the presence of minor populations of other oligomers. The significant dominance of octamers in the supersaturated solution indicates that they are elementary building blocks for the growth of KDP crystals of tetragonal modification. |
| first_indexed | 2024-03-09T13:06:42Z |
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| institution | Directory Open Access Journal |
| issn | 2073-4352 |
| language | English |
| last_indexed | 2024-03-09T13:06:42Z |
| publishDate | 2022-12-01 |
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| series | Crystals |
| spelling | doaj.art-6da4dc70b2514cf2b6717f8930571e9d2023-11-30T21:46:58ZengMDPI AGCrystals2073-43522022-12-011312610.3390/cryst13010026Temperature Behavior of Precursor Clusters at the Pre-Crystallization Phase of K(H<sub>2</sub>PO<sub>4</sub>) Studied by SAXSAndrey E. Sukhanov0Kseniia B. Ilina1Petr V. Konarev2Georgy S. Peters3Yury V. Pisarevsky4Ekaterina S. Smirnova5Olga A. Alekseeva6Mikhail V. Kovalchuk7A.V. Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics”, Russian Academy of Sciences, 59, Leninskii Prospect, Moscow 119333, RussiaA.V. Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics”, Russian Academy of Sciences, 59, Leninskii Prospect, Moscow 119333, RussiaA.V. Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics”, Russian Academy of Sciences, 59, Leninskii Prospect, Moscow 119333, RussiaNational Research Centre “Kurchatov Institute”, 1, Akademika Kurchatova Pl., Moscow 123182, RussiaA.V. Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics”, Russian Academy of Sciences, 59, Leninskii Prospect, Moscow 119333, RussiaA.V. Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics”, Russian Academy of Sciences, 59, Leninskii Prospect, Moscow 119333, RussiaA.V. Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics”, Russian Academy of Sciences, 59, Leninskii Prospect, Moscow 119333, RussiaA.V. Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics”, Russian Academy of Sciences, 59, Leninskii Prospect, Moscow 119333, RussiaElementary building blocks for the growth of KDP crystals were established. The solution of potassium dihydrogen phosphate (KH2PO4–KDP) has been experimentally studied by the small-angle X-ray scattering (SAXS) method. The analysis of SAXS data in the temperature range of 2.5–90 °C using a set of models of 3D fragments of the crystal structure showed that the saturated solution contains above K<sup>+</sup>, H<sub>2</sub>PO<sub>4</sub><sup>−</sup> and KH<sub>2</sub>PO<sub>4</sub> monomers, as well as mainly octamers. The 3D model of the octamer isolated from the crystal structure has dimensions of 17.443 Å along the [001] axis and 5.963 Å along the [100] and [010] axes. As the temperature is decreased, starting from the saturation temperature of the solution, the volume fraction of octamers sharply increases while the volume fraction of monomers decreases. The results indicate that the monomers and octamers represent major components in the solution with the presence of minor populations of other oligomers. The significant dominance of octamers in the supersaturated solution indicates that they are elementary building blocks for the growth of KDP crystals of tetragonal modification.https://www.mdpi.com/2073-4352/13/1/26three-stage crystallization modelprecursor clusterswater solutionsmall angle X-ray scatteringKDPsaturation |
| spellingShingle | Andrey E. Sukhanov Kseniia B. Ilina Petr V. Konarev Georgy S. Peters Yury V. Pisarevsky Ekaterina S. Smirnova Olga A. Alekseeva Mikhail V. Kovalchuk Temperature Behavior of Precursor Clusters at the Pre-Crystallization Phase of K(H<sub>2</sub>PO<sub>4</sub>) Studied by SAXS Crystals three-stage crystallization model precursor clusters water solution small angle X-ray scattering KDP saturation |
| title | Temperature Behavior of Precursor Clusters at the Pre-Crystallization Phase of K(H<sub>2</sub>PO<sub>4</sub>) Studied by SAXS |
| title_full | Temperature Behavior of Precursor Clusters at the Pre-Crystallization Phase of K(H<sub>2</sub>PO<sub>4</sub>) Studied by SAXS |
| title_fullStr | Temperature Behavior of Precursor Clusters at the Pre-Crystallization Phase of K(H<sub>2</sub>PO<sub>4</sub>) Studied by SAXS |
| title_full_unstemmed | Temperature Behavior of Precursor Clusters at the Pre-Crystallization Phase of K(H<sub>2</sub>PO<sub>4</sub>) Studied by SAXS |
| title_short | Temperature Behavior of Precursor Clusters at the Pre-Crystallization Phase of K(H<sub>2</sub>PO<sub>4</sub>) Studied by SAXS |
| title_sort | temperature behavior of precursor clusters at the pre crystallization phase of k h sub 2 sub po sub 4 sub studied by saxs |
| topic | three-stage crystallization model precursor clusters water solution small angle X-ray scattering KDP saturation |
| url | https://www.mdpi.com/2073-4352/13/1/26 |
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