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Updated: Jan 23, 2026

Optimization of Crystal Growth for Neutron Macromolecular Crystallography
Published on: March 13, 2021
Qualitative analysis on crystal growth of synthetic hydroxyapatite influenced by fluoride concentration
Sumi Kang1, Jeong Taeg Seo2, Sung-Ho Park1
1Department of Conservative Dentistry and Oral Science Research Center, College of Dentistry, Yonsei University, 50 Yonsei-ro, Seodaemun-gu, Seoul 120-752, Republic of Korea.
Objective:
This study was designed to analyze the crystal growth of synthetic hydroxyapatite (HA) particles in pH 7.0 supersaturated solutions with different fluoride concentrations by FE-SEM, FE-TEM, X-ray diffraction (XRD), and FTIR.
Design:
Eight groups of pH 7.0 calcium phosphate supersaturated solutions were prepared with different fluoride concentrations (0, 1, 2, 4, 8, 16, 32, and 64 ppm). Each solution was introduced into the reactive column containing the synthetic HA for 48 h. The resulting products were prepared for FE-SEM, FE-TEM, XRD, and FTIR.
Results:
The FE-SEM examination revealed various morphological changes of the crystals, with additional, less-ordered crystallites in experimental solutions containing more than 8 ppm of fluoride. FE-TEM examination showed an additional amorphous layer on the surface of the crystals with the presence of fluoride, whereas definite lattice structures completely reached the surface of the crystals without fluorides. XRD data showed that all crystals had the same patterns as the unreacted synthetic HA, regardless of fluoride concentration. With FTIR results, the intensity of the OH-libration mode decreased when adding fluoride, compared to that of pristine HA. The resulting crystals were considered to be partially fluoridated HA under room temperature and pH 7.0 supersaturated solutions.
Conclusion:
Under the experimental conditions in this study, fluorides mainly react with the surface of the seed HA and have an impact on the growth of HA in a less effective manner as the concentration of fluoride increases.
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