王家琪,白玉,李婷,高元明,马文.氟硒双掺羟基磷灰石涂层体外矿化性能及抗菌性能研究[J].表面技术,2024,53(18):210-218.
WANG Jiaqi,BAI Yu,LI Ting,GAO Yuanming,MA Wen.Vitro Mineralization and Antibacterial Properties of Fluoro-selenium Double-doped Hydroxyapatite Coating[J].Surface Technology,2024,53(18):210-218 |
| 氟硒双掺羟基磷灰石涂层体外矿化性能及抗菌性能研究 |
| Vitro Mineralization and Antibacterial Properties of Fluoro-selenium Double-doped Hydroxyapatite Coating |
| 投稿时间：2023-10-12 修订日期：2023-12-29 |
| DOI：10.16490/j.cnki.issn.1001-3660.2024.18.019 |
| 中文关键词: 生物涂层 氟硒双掺羟基磷灰石 矿化性能 矿化过程 抗菌性能 悬浮液等离子喷涂 |
| 英文关键词:biological coating fluoro-seleno-hydroxyapatite mineralization property mineralization process antibacterial property suspension plasma spraying |
| 基金项目:国家自然科学基金项目(52062041);内蒙古自然科学基金项目(2022MS05003);内蒙古自治区高等学校青年科技人才发展计划项目(NJYT22080，NMGIRT2319);内蒙古自治区直属高校基本科研业务费(JY20220062，JY20220041) |
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| Author | Institution |
| WANG Jiaqi | Inner Mongolia Key Laboratory of Thin Film and Coating, School of Materials Science and Engineering, Inner Mongolia University of Technology, Hohhot 010051, China |
| BAI Yu | Inner Mongolia Key Laboratory of Thin Film and Coating, School of Materials Science and Engineering, Inner Mongolia University of Technology, Hohhot 010051, China |
| LI Ting | Inner Mongolia Key Laboratory of Thin Film and Coating, School of Materials Science and Engineering, Inner Mongolia University of Technology, Hohhot 010051, China |
| GAO Yuanming | Inner Mongolia Key Laboratory of Thin Film and Coating, School of Materials Science and Engineering, Inner Mongolia University of Technology, Hohhot 010051, China |
| MA Wen | Inner Mongolia Key Laboratory of Thin Film and Coating, School of Materials Science and Engineering, Inner Mongolia University of Technology, Hohhot 010051, China |
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| 中文摘要: |
| 目的 制备一种具有抗菌能力和骨骼矿化能力的HA涂层，探究在Se/P(物质的量比)为0.15时，不同掺F量对涂层抗菌能力和矿化能力的影响。方法 采用共沉淀法制备F、Se共掺羟基磷灰石悬浮液(Se-F-HA)，经洗涤和过滤将其固含量调整至10%，通过悬浮液等离子喷涂技术(SPS)，在医用金属钛表面沉积Se-F-HA涂层，通过XRD、XPS、SEM-EDS对涂层进行表征。以体外矿化实验和抗菌实验评价涂层矿化能力和抗菌能力。结果 XRD表明3种涂层均为HA相，F、Se并未引起HA相变;EDS和XPS表明F、Se成功进入HA晶格，元素并未发生明显氧化。矿化实验表明，随着掺F量的增加，涂层失重减少，形成矿化层速率加快，磷灰石密度增加。矿化5 d后Se-1.5FHA涂层增重0.013 g/cm2，矿化后3种涂层Ca/(Se+P)(物质的量比)值均高于1.67，表明涂层表面吸附Ca2+、PO43–，形成Ca/P(物质的量比)大于1.67的磷灰石层。抗菌实验表明，Se-F-HA涂层对细菌增殖起到明显的抑制作用。结论 F、Se可以促进HA涂层的矿化，F可以有效降低SeHA溶解度。Se-FHA涂层对金黄色葡萄球菌的增殖起到明显抑制作用，相较于HA组，Se-1.5FHA组细菌数量下降了近2个数量级，为骨缺损提供了具有良好抗菌能力和骨骼矿化能力的材料。 |
| 英文摘要: |
| The work aims to prepare fluorine and selenium-doped hydroxyapatite nano-powder suspension by hydrothermal coprecipitation method and apply the co-doped hydroxyapatite coating on the surface of titanium substrate by suspension. By suspension plasma spraying technology, this short coating preparation process avoids drying, grinding powder and some other steps. Due to the weak antibacterial properties of hydroxyapatite, it is difficult to meet the requirements of medical applications. In this work, the effects of fluorine and selenium doping on the antibacterial activity and mineralization ability of the coating are studied. 0.7 mol/L aqueous solution was prepared by calcium nitrate tetrahydrate, diammonium hydrogen phosphate, ammonium fluoride and sodium selenite according to the stoichiometric ratio of hydroxyapatite. HA, Se-0.5FHA and Se-1.5FHA suspensions were prepared by coprecipitation method. The Se/P ratios of the three samples were 0, 15% and 15%, respectively. The F/ OH ratios were 0, 0.3 and 3, respectively. At 40 ℃, the solution of diammonium hydrogen phosphate, ammonium fluoride, sodium selenite was mixed and slowly added to calcium nitrate tetrahydrate. The titanium substrate (10 mm×10 mm× 2 mm) was sandblasted to increase the surface roughness, and then plasma sprayed with suspension by MC 60 spray gun (Medicoat AG, Switzerland). During the spraying process, the distance between the nozzle and the substrate surface was 40 mm, the transverse moving speed was 700 mm/s, and the longitudinal step length was 150 mm. After 20 layers of spraying, the coating thickness was maintained at about 80 um. The coatings were characterized by XRD, XPS and SEM-EDS. XRD analysis revealed that the coating was primarily composed of HA phase, with some products decomposing to form a small amount of α-TCP, β-TCP and TTCP during spraying. XPS analysis indicated that F- replaced OH- and SeO32– replaced PO43– into the lattice. The surface scan by EDS results showed that the coating contained Ca, P, Se, F and other elements, and Ca/ (Se + P) conformed to the stoichiometric ratio of hydroxyapatite, which was stable at about 1.67. The mineralization ability was evaluated by measuring the weight gain and pH change of the coating before and after immersion in simulated body fluid (SBF). Because the incorporation of Se element into HA might increase lattice expansion and solubility, the crystals tended to stabilize with the increase of F content, and the formation rate of HA mineralized layer accelerated. After 5 d of mineralization, the weight gain of Se-1.5FHA coating was up to 0.013 g/cm2, and the EDS spectra showed that Ca/(Se + P) after mineralization was higher than 1.67, indicating that Ca2+ and PO43– were absorbed on the surface of the coating, and an apatite layer with Ca/P greater than 1.67 was formed. Bacterial culture experiments using staphylococcus aureus suspension showed that the absorbance of the coating with F and Se elements was much lower than that of the HA group and was consistent with the law of colony growth. Doping F and Se elements can improve the mineralization effect of HA coating and avoid the dissolution of HA caused by single Se. Compared with the HA coating, the number of bacteria in the doped samples decreases by about two orders of magnitude, providing an implant material with good bacteriostatic and mineralization ability for bone defects. |
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