A microwave-assisted hydrothermal method for rapidly synthesizing nanocrystalline carbonated hydroxyapatite from calcium resources in crab shell waste

Next Materials Pub Date : 2025-07-22 DOI:10.1016/j.nxmate.2025.100946

Yustina M. Pusparizkita , Roihan A. Faizal , Samsul A. Perwira Negara , Rifky Ismail , J. Jamari , Athanasius P. Bayuseno

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Abstract

Nanocrystalline carbonated hydroxyapatite (CHA) shows significant promise for bone replacement within biomedical applications. This study aimed to synthesize nanocrystalline CHA using calcium resources from crab shell waste through a microwave-assisted hydrothermal technique. In this way, the crab shells were initially pulverized and calcined at 900° C for 5 h, yielding Ca(OH)₂ powder. This powder was then dissolved in a prepared hydrothermal solution of diammonium phosphate and subjected to microwave irradiation for 3 min at power levels of 80, 240, and 400 watt. X-ray diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) analyses confirmed the nanocrystalline CHA type B formed with a crystallinity index ranging from 79 % to 99.5 %. SEM images show the agglomerated morphology (0.5 μm-1 μm) of nanocrystalline CHA, with crystallite sizes ranging from 15 nm to 17 nm. Recycling calcium biogenic sources from crab shells as a powder feedstock using microwave-assisted synthesis is a rapid and environmentally friendly method for producing nanocrystalline CHA powder, which has potential applications in biomedical materials due to its high bioactivity and adsorption capacity.

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微波辅助水热法从蟹壳废钙资源中快速合成纳米晶碳化羟基磷灰石

纳米晶碳化羟基磷灰石（CHA）在生物医学应用中显示出重要的骨替代前景。本研究旨在利用蟹壳废弃物中的钙资源，通过微波辅助水热技术合成纳米晶CHA。通过这种方法，将蟹壳粉碎，在900℃下煅烧5 h，得到Ca(OH) 2粉末。然后将该粉末溶解在制备好的磷酸二铵水热溶液中，并在80、240和400瓦的功率下进行3 min的微波照射。x射线衍射（XRD）和傅里叶变换红外光谱（FTIR）分析证实形成了CHA B型纳米晶，结晶度指数为79 % ~ 99.5 %。SEM图像显示纳米晶CHA的团聚形貌（0.5 μm-1 μm），晶粒尺寸在15 ~ 17 nm之间。利用微波辅助合成技术回收蟹壳中生物源钙作为粉末原料是一种快速、环保的制备纳米晶CHA粉末的方法，其具有较高的生物活性和吸附能力，在生物医学材料中具有潜在的应用前景。

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