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蛋壳衍生羟基磷灰石在宽烧结温度范围内的相变与力学优化

Phase Transformation and Mechanical Optimization of Eggshell-Derived Hydroxyapatite across a Wide Sintering Temperature Range.

作者信息

Wu Shih-Ching, Hsu Hsueh-Chuan, Liu Mei-Yi, Ho Wen-Fu

机构信息

Department of Dental Technology and Materials Science, Central Taiwan University of Science and Technology, Taichung 406053, Taiwan.

Department of Materials Science and Engineering, Da-Yeh University, Changhua 515006, Taiwan.

出版信息

Materials (Basel). 2024 Aug 15;17(16):4062. doi: 10.3390/ma17164062.

Abstract

Calcium phosphate, particularly hydroxyapatite (HA), bears a close resemblance to human bones, rendering it a prevalent material in biomedical applications. This study focuses on the successful preparation of HA using a precipitation method with eggshell as a raw material. Subsequently, the HA powder was press-formed and sintered at various temperatures to investigate the impact of sintering temperature on the mechanical properties, including hardness, compressive strength, and fracture toughness, of the sintered HA samples (E-HA). Statistical analyses, including one-way ANOVA and Tukey's post-hoc test, were conducted to determine significant differences in these properties at different sintering temperatures. Experimental findings revealed that as the sintering temperature increased, HA partially transformed into β-TCP between 800 and 1300 °C, with α-TCP observed at 1400 °C. The elimination of pores led to an increase in relative density, with a maximum relative density of 94.5% achieved at 1200 and 1300 °C. E-HA sintered at 1200 °C exhibited the highest hardness (5.08 GPa), compressive strength (255.79 MPa), and fracture toughness (1.21 MPa·m0.5). However, at 1400 °C, a slight decrease in apparent density (2.90 g/cm) was noted due to the presence of α-TCP, along with significant grain growth. This study's objective is clearly aligned with the study design, incorporating detailed statistical analyses to validate the findings. Furthermore, bacterial culture experiments were conducted using sintered E-HA, Chem-HA (HA synthesized from reagent-grade calcium carbonate), and Comm-HA (commercial HA). was cultured on the surfaces of sintered E-HA, Chem-HA, and Comm-HA samples for 20 h. After culturing, the OD values for all samples were below 0.2, indicating significant antibacterial efficacy. The comparable OD values and bacterial counts ( > 0.05) suggest that the source of HA does not impact its antibacterial properties. This underscores the potential of eggshell-derived HA as an effective material for biomedical applications.

摘要

磷酸钙,尤其是羟基磷灰石(HA),与人体骨骼极为相似,这使其成为生物医学应用中一种普遍使用的材料。本研究聚焦于以蛋壳为原料,通过沉淀法成功制备HA。随后,将HA粉末进行压制成型,并在不同温度下烧结,以研究烧结温度对烧结HA样品(E-HA)的机械性能(包括硬度、抗压强度和断裂韧性)的影响。进行了包括单因素方差分析和Tukey事后检验在内的统计分析,以确定在不同烧结温度下这些性能的显著差异。实验结果表明,随着烧结温度升高,HA在800至1300℃之间部分转变为β-TCP,在1400℃时观察到α-TCP。孔隙的消除导致相对密度增加,在1200和1300℃时达到最大相对密度94.5%。在1200℃烧结的E-HA表现出最高的硬度(5.08 GPa)、抗压强度(255.79 MPa)和断裂韧性(1.21 MPa·m0.5)。然而,在1400℃时,由于α-TCP的存在以及明显的晶粒生长,表观密度略有下降(2.90 g/cm)。本研究的目标与研究设计明确一致,纳入了详细的统计分析以验证研究结果。此外,使用烧结的E-HA、化学合成HA(由试剂级碳酸钙合成的HA)和商业HA进行了细菌培养实验。在烧结的E-HA、化学合成HA和商业HA样品表面培养20小时。培养后,所有样品的OD值均低于0.2,表明具有显著的抗菌效果。可比的OD值和细菌计数(>0.05)表明HA的来源不影响其抗菌性能。这突出了蛋壳衍生HA作为生物医学应用有效材料的潜力。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/b7b0/11356715/3fc2325d4f63/materials-17-04062-g001.jpg

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