Hydroxyapatite nanoparticles produced by direct precipitation method: Optimization and characterization studies
Hydroxyapatite nanoparticles produced by direct precipitation method: Optimization and characterization studies
复制标题
直接沉淀法生产的羟基磷灰石纳米粒子：优化和表征研究
DOI：
10.1063/5.0044252
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发表时间：
2021
期刊：
影响因子：
--
通讯作者：
M. N. Salimi
中科院分区：
文献类型：
--
作者：
Hor Wee Fern;M. N. Salimi
羟基磷灰石(HAP)，[Ca10(PO4)6(OH)2]的需求量越来越大，在生物医学领域得到了广泛的应用。对直接沉淀法制备羟基磷灰石纳米粒子进行了优化和表征研究。以氢氧化钙[Ca(OH)2]和磷酸(H3PO4)为前驱体，溶解在蒸馏水中，经过滤、干燥、研磨等步骤制得白色沉淀的干粉。采用响应面方法和中心组合设计法研究了不同加工温度(30~50˚C)、搅拌时间(30~60 )和搅拌速度(300~500 rpm)对羟基磷灰石微晶尺寸的影响。经方差分析，确定系数R2为0.8736，其中加工温度是影响羟基磷灰石微晶尺寸的变量。利用设计专家软件对羟基磷灰石的制备进行了优化，在35℃、400 转速下反应45分钟，得到了最小的微晶尺寸为0.2990 nm的羟基磷灰石。采用傅立叶变换红外光谱仪(FTIR)、X射线衍射仪(X射线衍射仪)、扫描电子显微镜(SEM)等分析手段对HAP粉末样品进行了表征。红外光谱分析表明，样品中含有磷酸(PO3-−)、羟基(OH-−)和碳酸盐(CO2-−)基团。在2θ=26°处的特征峰表明样品中存在羟基磷灰石。在较低搅拌速度下，颗粒呈长方体状，较高搅拌速度下，颗粒呈拉长椭圆形。
Hydroxyapatite (HAp), [Ca10(PO4)6(OH)2] has been increasingly in demand and extensively used in biomedical field. Optimization and characterization studies were carried out on the production of HAp nanoparticles by direct precipitation method. Calcium hydroxide [Ca(OH)2] and orthophosphoric acid (H3PO4) were used as precursors which are dissolved in distilled water followed by filtration, drying and grinding processes in order to obtain a dried white precipitated HAp powder. The effect of different processing temperatures (30 to 50 ˚C), stirring time (30 to 60 min) and stirring rates (300 to 500 rpm) towards the crystallite size of HAp were investigated by using Response Surface Methodology (RSM) and Central Composite Design (CCD). Based on analysis of variance (ANOVA), the determination coefficient, R2 obtained was 0.8736 where processing temperature was the influential variable on crystallite size of HAp. Design Expert Software (DOE) was used to optimize the production of HAp and the smallest crystallite size of HAp with 0.2990 nm was obtained based on the optimum condition at 35 °C for 45 minutes with 400 rpm. The characterization of the HAp powder samples were evaluated by using different analytical tools such as Fourier Transform Infrared Spectrometer (FTIR), X-Ray Diffractometer (XRD) and Scanning Electron Microscope (SEM). Phosphate (PO 3−), hydroxyl (OH−) and carbonate (CO 2−) groups were identified in the FTIR spectra pattern of samples. The characteristic peak occurring at 2θ=26° indicated the presence of HAp in the samples. The particles appeared as agglomerates and were generally cuboid-like at a lower stirring rate and elongated ellipse-like appearance at the higher stirring rate.