多孔ZnO-MgO/羟基磷灰石复合材料的制备与体外生物学性能

王淇; 朱斌; 罗丽琳; 孟增东; 张玉勤

doi:10.13801/j.cnki.fhclxb.20220105.003

多孔ZnO-MgO/羟基磷灰石复合材料的制备与体外生物学性能

doi: 10.13801/j.cnki.fhclxb.20220105.003

王淇^1,,
朱斌¹,
罗丽琳²,
孟增东³,
张玉勤^1, ,

1.
昆明理工大学　材料科学与工程学院，昆明 650093
2.
云南省第一人民医院　病理科，昆明 650032
3.
云南省第一人民医院　骨科，昆明 650032

基金项目: 国家自然科学基金(31860264)；云南省基础研究计划重点项目(2019FA029)

详细信息

通讯作者:
张玉勤，博士，教授，博士生导师，研究方向为生物医用材料　E-mail: zyqkust@163.com

中图分类号: TB332
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出版历程
- 收稿日期: 2021-11-02
- 修回日期: 2021-12-23
- 录用日期: 2021-12-26
- 网络出版日期: 2022-01-06
- 刊出日期: 2022-12-01

Preparation and in vitro biological properties of porous ZnO-MgO/hydroxyapatite biocomposites

1.
School of Materials Science and Engineering, Kunming University of Science and Technology, Kunming 650093, China
2.
First People's Hospital of Yunnan Province, Department of Pathology, Kunming 650032, China
3.
First People's Hospital of Yunnan Province, Department of Orthopedics, Kunming 650032, China

摘要

摘要: 为改善多孔羟基磷灰石(HA)生物复合材料的生物活性和成骨诱导能力，本文利用放电等离子烧结(SPS)技术制备了ZnO、MgO质量分数分别为1.3wt%、8.4wt%的多孔ZnO-MgO/HA生物复合材料，研究了不同烧结温度下多孔复合材料微观结构、孔隙特征、体外矿化及降解行为的变化规律并对比分析了活性陶瓷相加入对多孔HA材料体外生物学性能的影响及机制。结果表明：烧结后的多孔复合材料主要由HA相及ZnO、MgO相组成，烧结温度超过950℃后，出现了少量HA分解产物Ca₃(PO₄)₂相；随烧结温度的升高，多孔复合材料孔隙率缓慢下降，孔径尺寸呈逐渐减小的趋势；不同烧结温度下多孔复合材料在模拟体液中均具有良好的类骨磷灰石形成能力，而降解率随温度提高先增大后减小；综合分析，950℃下制备的多孔ZnO-MgO/HA复合材料具有适宜的孔隙特征(孔隙率(34.7±0.2)%，孔径尺寸150~400 μm占比65.5%)，同时与多孔HA材料相比，还具有优异的类骨磷灰石形成能力、高的降解率((11.3±0.2)%)和细胞增殖率((91.7±2.1)%)及低的细胞凋亡率((2.3±0.2)%)，表明ZnO和MgO活性陶瓷相的加入明显提高了多孔HA材料的成骨诱导能力与生物相容性。
- 多孔羟基磷灰石 /
- ZnO-MgO /
- 烧结温度 /
- 孔隙特征 /
- 生物相容性 /
- 放电等离子烧结(SPS)
Abstract: In order to improve the bioactivity and osteogenic induction ability of porous hydroxyapatite (HA) biocomposites, porous ZnO-MgO/HA biocomposites with the mass fraction of ZnO 1.3wt% and MgO 8.4wt% were prepared by spark plasma sintering (SPS). The changes of microstructure, pore characteristics, in vitro mineralization and degradation behavior of porous composites at different sintering temperatures were studied. The effect of active ceramic phase addition on biological properties of porous HA materials in vitro and its mechanism were analyzed. The results show that the sintered porous composites are mainly composed of HA, ZnO and MgO phase. When the sintering temperature exceeds 950℃, a small amount of HA decomposition product Ca₃(PO₄)₂ phase appears. With the increase of sintering temperature, the porosity of porous composites decreases slowly, and the pore size decreases gradually. The porous composites have good osteoapatite formation ability in simulated body fluid at different sintering temperatures, and the degradation rate increases first and then decreases with the increase of sintering temperature. Comprehensive analysis shows that the porous ZnO-MgO/HA composites prepared at 950℃ have suitable pore characteristics (porosity (34.7±0.2)%, pore size between 150-400 μm accounts for 65.5%). Moreover, the porous HA material has excellent osteogenic ability, high degradation rate ((11.3±0.2)%), high cell proliferation rate ((91.7±2.1)%) and low cell apoptosis rate ((2.3±0.2)%), indicating that the addition of ZnO and MgO active ceramic phase significantly improves the osteogenic induction ability and biocompatibility of porous HA material.
- porous hydroxyapatite /
- ZnO-MgO /
- sintering temperature /
- pore characteristics /
- biocompatibility /
- spark plasma sintering (SPS)

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图 1 不同温度烧结下多孔ZnO-MgO/羟基磷灰石(HA)复合材料XRD图谱

Figure 1. XRD patterns of porous ZnO-MgO/hydroxyapatite (HA) composites sintered at different temperatures

TCP—Ca₃(PO₄)₂

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图 2 不同烧结温度下多孔ZnO-MgO/HA复合材料纵切面形貌图及孔径尺寸分布图

Figure 2. Longitudinal section morphology and pore size distribution of porous ZnO-MgO/HA composites at different sintering temperatures

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图 3 不同烧结温度下多孔ZnO-MgO/HA复合材料在模拟人工体液溶液中浸泡14天后的表面生物矿化形貌图及EDS点扫描分析图

Figure 3. SEM and EDS point scanning analysis of porous ZnO-MgO/HA composites soaked in simulated artificial body fluid solution for 14 days at different sintering temperatures ((a) 850℃; (b) 900℃ (c); 950℃; (d) 1000℃; (e) 1050℃; (f) EDS point scanning analysis diagram at the marker)

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图 4 多孔HA材料在模拟人工体液溶液(SBF)中浸泡14天后的表面生物矿化SEM图像

Figure 4. SEM images of surface bio-mineralization of porous HA soaked in simulated artificial body fluid solution (SBF) for 14 days

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图 5 多孔ZnO-MgO/HA复合材料的体外矿化及降解机制

Figure 5. In vitro mineralization and degradation mechanism of porous ZnO-MgO/HA composites

SBF—Simulated artificial body fluid

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图 6 多孔HA材料及多孔ZnO-MgO/HA复合材料在模拟人工体液溶液中浸泡7周后降解率曲线

Figure 6. Degradation curves of porous HA materials and porous ZnO-MgO/HA composites soaked in simulated artificial body fluid solution for 7 weeks

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图 7 不同培养时间下多孔HA材料及多孔ZnO-MgO/HA复合材料表面的MG63细胞增殖

Figure 7. MG63 cell proliferation on the surface of porous HA material and porous ZnO-MgO/HA composite under different incubation time (*—Significant difference value (P)<0.05; **—P<0.01)

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图 8 多孔HA材料(a)及多孔ZnO-MgO/HA复合材料(b)浸提液诱导MG63细胞凋亡散点统计图

Figure 8. Scatterplot of apoptosis induced by porous HA material (a) and porous ZnO-MgO/HA composite (b) extract of MG63 cells

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图 9 多孔HA材料及多孔ZnO-MgO/HA复合材料浸提液诱导MG63细胞凋亡率(*—P<0.05)

Figure 9. Statistical diagram of apoptosis rate of MG63 cells induced by porous HA material and porous ZnO-MgO/HA composite extract (*—P<0.05)

下载: 全尺寸图片幻灯片

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