Synthesis, Characterization and Process Optimization of Bone Whitlockite
Whitlockite, being the second most abundant bio-mineral in living bone, finds huge applications in tissue regeneration and implants and its synthesis into its pure form has remained a challenge. Although precipitation of whitlockite phase has been reported recently in many publications, effects of v...
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| Format: | Article |
| Language: | English |
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MDPI AG
2020-09-01
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| Series: | Nanomaterials |
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| Online Access: | https://www.mdpi.com/2079-4991/10/9/1856 |
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| author | Sadaf Batool Usman Liaqat Zakir Hussain Manzar Sohail |
| author_facet | Sadaf Batool Usman Liaqat Zakir Hussain Manzar Sohail |
| author_sort | Sadaf Batool |
| collection | DOAJ |
| description | Whitlockite, being the second most abundant bio-mineral in living bone, finds huge applications in tissue regeneration and implants and its synthesis into its pure form has remained a challenge. Although precipitation of whitlockite phase has been reported recently in many publications, effects of various parameters to control such phase as well as conditions for the bulk preparation of this extremely important bio-mineral have not been investigated so far. In this work, we report the precipitation of pure whitlockite phase using common precursors. As reported in the literature, whitlockite is stable in a narrow pH range, therefore; optimization of pH for the stabilization of whitlockite phase has been investigated. Additionally, in order to narrow down the optimum conditions for the whitlockite precipitation, effect of temperature and heating conditions has also been studied. The obtained solids were characterized using powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). From PXRD analysis, it was observed that heating the precursor’s mixture at 100 °C with subsequent aging at the optimized pH resulted in the precipitation of pure whitlockite phase. These results were further confirmed by TGA, SEM and Raman spectroscopy analysis and it was confirmed that the conditions reported here favor whitlockite precipitation without formation of any secondary phase. These reaction conditions were further confirmed by changing all the parameters like aging, heating time, feed rate of precursors one by one. From PXRD analysis of these samples, it was concluded that not only pH but temperature, heating time, aging time and feed rate effect simultaneously on the precipitation of pure whitlockite phase and a subtle change in any of these parameters could lead to the formation of undesired stable secondary calcium phosphate phases. |
| first_indexed | 2024-03-10T16:16:57Z |
| format | Article |
| id | doaj.art-7b3bbad5eefc43ba87daa8c485e71704 |
| institution | Directory Open Access Journal |
| issn | 2079-4991 |
| language | English |
| last_indexed | 2024-03-10T16:16:57Z |
| publishDate | 2020-09-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Nanomaterials |
| spelling | doaj.art-7b3bbad5eefc43ba87daa8c485e717042023-11-20T14:00:12ZengMDPI AGNanomaterials2079-49912020-09-01109185610.3390/nano10091856Synthesis, Characterization and Process Optimization of Bone WhitlockiteSadaf Batool0Usman Liaqat1Zakir Hussain2Manzar Sohail3School of Chemical and Materials Engineering (SCME), National University of Sciences & Technology (NUST), Sector H-12, 44000 Islamabad, PakistanSchool of Chemical and Materials Engineering (SCME), National University of Sciences & Technology (NUST), Sector H-12, 44000 Islamabad, PakistanSchool of Chemical and Materials Engineering (SCME), National University of Sciences & Technology (NUST), Sector H-12, 44000 Islamabad, PakistanDepartment of Chemistry, School of Natural Sciences (SNS), National University of Sciences & Technology (NUST), Sector H-12, 44000 Islamabad, PakistanWhitlockite, being the second most abundant bio-mineral in living bone, finds huge applications in tissue regeneration and implants and its synthesis into its pure form has remained a challenge. Although precipitation of whitlockite phase has been reported recently in many publications, effects of various parameters to control such phase as well as conditions for the bulk preparation of this extremely important bio-mineral have not been investigated so far. In this work, we report the precipitation of pure whitlockite phase using common precursors. As reported in the literature, whitlockite is stable in a narrow pH range, therefore; optimization of pH for the stabilization of whitlockite phase has been investigated. Additionally, in order to narrow down the optimum conditions for the whitlockite precipitation, effect of temperature and heating conditions has also been studied. The obtained solids were characterized using powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). From PXRD analysis, it was observed that heating the precursor’s mixture at 100 °C with subsequent aging at the optimized pH resulted in the precipitation of pure whitlockite phase. These results were further confirmed by TGA, SEM and Raman spectroscopy analysis and it was confirmed that the conditions reported here favor whitlockite precipitation without formation of any secondary phase. These reaction conditions were further confirmed by changing all the parameters like aging, heating time, feed rate of precursors one by one. From PXRD analysis of these samples, it was concluded that not only pH but temperature, heating time, aging time and feed rate effect simultaneously on the precipitation of pure whitlockite phase and a subtle change in any of these parameters could lead to the formation of undesired stable secondary calcium phosphate phases.https://www.mdpi.com/2079-4991/10/9/1856whitlockitebone mineralcalcium phosphatesynthesisprocess optimization |
| spellingShingle | Sadaf Batool Usman Liaqat Zakir Hussain Manzar Sohail Synthesis, Characterization and Process Optimization of Bone Whitlockite Nanomaterials whitlockite bone mineral calcium phosphate synthesis process optimization |
| title | Synthesis, Characterization and Process Optimization of Bone Whitlockite |
| title_full | Synthesis, Characterization and Process Optimization of Bone Whitlockite |
| title_fullStr | Synthesis, Characterization and Process Optimization of Bone Whitlockite |
| title_full_unstemmed | Synthesis, Characterization and Process Optimization of Bone Whitlockite |
| title_short | Synthesis, Characterization and Process Optimization of Bone Whitlockite |
| title_sort | synthesis characterization and process optimization of bone whitlockite |
| topic | whitlockite bone mineral calcium phosphate synthesis process optimization |
| url | https://www.mdpi.com/2079-4991/10/9/1856 |
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