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Nanostructures of Hydroxyapatite in Pluronic F 127: Preparation and Structural Characterization

机译:Pluronic F 127中羟基磷灰石的纳米结构:制备与结构表征

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In this work, nanocomposites of hydroxyapatite and Pluronic F127 were prepared by a wet chemical method, using acid-basic reaction with Ca/P ratio of 1.67 in 10% (m/V) Pluronic F127 at 0, 37 and 90℃. The final concentration of Pluronic F127 was adjusted to 37% (m/V) at 4℃. Afterwards, the samples were lyophilized. Characterization was performed in purified samples (after Pluronic F127 removal), samples with 10% (m/V) of Pluronic F127 and calcined samples at 1000℃ by X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscopy (SEM). Analyses by XRD of non-calcined samples showed that hydroxyapatite was obtained, in which the samples prepared at 0℃ exhibited larger peaks attributed to lower crystallite sizes. For the calcined samples, both Raman spectroscopy and XRD exhibited hydroxyapatite for the syntheses at 37 and 90℃ whereas the one prepared 90℃ were identified as P-tricalcium phosphate (β-TCP). Morphological analysis by SEM indicated that the hydroxyapatite was sphere or rod agglomerates in mesoporous morphology for the nanocomposites prepared at 0 and 37℃, while the sample prepared at 90℃ was nanospheres agglomerated into a smother matrix. After Pluronic F127 removal, samples fabricated at 0 and 37 ℃ exhibited coalescence of the nanostructures, whereas the sample synthesized at 90℃ kept mesoporous. Calcined samples showed sintering and some rods structures.
机译:在这项工作中,通过湿化学法制备羟基磷灰石和Pluronic F127的纳米复合材料,在10%(m / V)Pluronic F127中,在0、37和90℃下,采用Ca / P比为1.67的酸碱反应。在4℃下将Pluronic F127的最终浓度调整为37%(m / V)。之后,将样品冻干。通过X射线衍射(XRD),拉曼光谱和扫描电子显微镜(SEM)在纯化的样品(去除Pluronic F127之后),含10%(m / V)Pluronic F127的样品和煅烧样品中进行表征。用XRD对未煅烧样​​品进行分析表明,获得了羟基磷灰石,其中0℃下制备的样品具有较大的峰,这归因于较低的晶粒尺寸。对于煅烧后的样品,拉曼光谱和XRD均显示在37和90℃合成羟基磷灰石,而制备的90℃鉴定为P-磷酸三钙(β-TCP)。扫描电镜(SEM)的形态分析表明,在0℃和37℃下制备的纳米复合材料中,羟基磷灰石为中孔形的球形或棒状团聚体,而在90℃下制备的样品是在球形基质中团聚而成的。去除Pluronic F127后,在0和37℃下制备的样品表现出纳米结构的聚结,而在90℃下合成的样品保持中孔。煅烧样品显示出烧结和一些棒状结构。

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