CN114931664B - 一种均匀降解的功能锌合金多孔骨支架及其制备方法 - Google Patents

一种均匀降解的功能锌合金多孔骨支架及其制备方法 Download PDF

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CN114931664B
CN114931664B CN202210593350.8A CN202210593350A CN114931664B CN 114931664 B CN114931664 B CN 114931664B CN 202210593350 A CN202210593350 A CN 202210593350A CN 114931664 B CN114931664 B CN 114931664B
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陈莉莉
赵丹雷
王佳佳
唐清明
魏青松
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Tongji Medical College of Huazhong University of Science and Technology
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Abstract

本发明公开了一种均匀降解的功能锌合金多孔骨支架及其制备方法，涉及医用生物材料技术领域。本发明所述多孔骨支架以Zn‑Mg‑X合金为基材，其中Mg元素含量为3‑20wt.％，X元素含量为1‑5wt.％，余量为Zn元素；所述X元素为Cu、Fe或Ag中的一种，然后通过激光选区熔化技术制备Zn合金多孔骨支架。本发明所制备的多孔骨支架不仅首次通过构建X/Zn和Zn/Mg双重微电池实现了多孔支架的均匀降解，还可通过释放功能金属离子持续为骨组织重建提供免疫介导成骨和抑菌抗感染的环境，有效解决现有可降解金属多孔支架缺乏降解均匀性与功能性的问题，工艺简单，应用前景广阔。

Description

一种均匀降解的功能锌合金多孔骨支架及其制备方法
技术领域
本发明属于医用生物材料技术领域，具体涉及一种均匀降解的功能锌合金多孔骨支架及其制备方法。
背景技术
大段骨缺损修复是临床面临的重大挑战。随着技术发展，骨植入体从早期的仅需提供支撑，将转向诱导骨缺损再生，重塑骨组织。可降解Zn合金具有良好的力学性能与可降解性，能够提供足够力学支撑，完成修复后还能自行降解消失，实现植入体向健全骨组织的完全转化。
实现骨组织再生关键在于，首先提供三维联通的多孔网络，为骨细胞提供立体生长环境，同时具备促骨生长，抑菌抗感染的能力。在修复过程中，还需保持降解均匀性，避免植入体提前失效。然而，现有研究中，控制降解和提供功能性主要通过制备涂层，一方面，现在涂层技术难以在具有复杂精细结构的3D打印多孔骨支架的表面构建均匀致密的涂层，另一方面当支架开始降解后，涂层服役失效，降解均匀性与功能性随之消失，进而无法在骨修复整个过程中提供降解均匀性与功能性。因此提供一种均匀降解的功能锌合金多孔骨支架是临床迫切需求。
发明内容
针对上述问题，本发明提供了一种均匀降解的功能锌合金多孔骨支架及其制备方法。
本发明所述均匀降解的功能Zn合金多孔骨支架为Zn-Mg-X合金，其中Mg元素含量为3-20wt.％，X元素含量为1-5wt.％，余量为Zn元素；所述X元素为Cu、Fe或Ag中的一种；所述多孔骨支架中构建有X/Zn和Zn/Mg双重微电池，具有降解均匀、抗菌和免疫诱导成骨的能力。
本发明所述均匀降解的功能锌合金多孔骨支架的制备方法包括以下步骤：
(1)按比例称取Zn粉、X粉和Mg粉，在氩气保护下进行球磨混合得到Zn-Mg-X合金粉末；
(2)将三维联通多孔结构模型导入激光选区熔化设备，然后将Zn-Mg-X合金粉末进行激光选区熔化打印，得到多孔支架；
(3)将打印得到的多孔支架进行喷砂、超声处理，烘干后得到成品。
优选的，所述Zn粉、X粉和Mg粉均为球形，所述Zn粉和Mg粉粒径均为15-53μm；所述X粉粒径为10-30μm之间。
优选的，步骤(1)所述的球磨参数为250r/min，球磨时间为4h，同时在球磨过程中需要间歇1h防止粉末粘黏。
优选的，步骤(2)所述激光选区熔化打印参数如下：
激光功率为60-150W，扫描速度为400-700mm/s，扫描策略为层间旋转67度，基板预热100-150℃。
优选的，步骤(3)所述的超声处理是将多孔支架依次在去离子水、乙醇和丙酮中超声30min，直到无黑色金属粉末脱落。
与现有技术相比，本发明具有以下有益效果：
本发明利用激光选区熔化(SLM)技术制备一种具有双重微电池的Zn合金多孔骨支架。SLM具有独特的微熔池冶炼能力，熔池内部热对流与非平衡凝固可以有效促进合金元素在Zn基体中的均匀分布，从而得到均匀的X/Zn和Zn/Mg双重微电池。X元素由于具有最高的电极电位，可以促进Zn和Mg在同一阶段发生腐蚀降解，暨先发生Zn/Mg电池反应，Mg降解，再发生X/Zn电池反应，Zn降解，而X元素又会随Zn基体的脱落一起脱落，进而达到降解均匀的目的。
在降解过程中，合金元素Mg释放的Mg离子能够为支架提供通过免疫介导促进成骨的能力，X合金元素一方面通过释放X离子提供抗菌能力，另一方面促进均匀降解。与涂层相比，本发明可在整个降解周期中持续输出功能性，兼备抗菌与诱导成骨的功能。
本发明所用合金元素均具有生物相容性，用于提供抗菌的合金元素不会产生耐药性，可有效保持杀菌性，降解后可被细胞吞噬排出。
附图说明
图1为本发明实施例1Zn-Mg-Cu合金多孔骨支架的降解宏微观形貌；
图2为本发明实施例1Zn-Mg-Cu合金多孔支架与对比例2Zn-Mg合金多孔支架的降解形貌对比；
图3为本发明实施例1Zn-Mg-Cu合金多孔骨支架的抗菌性能；
图4为本发明实施例1所述功能Zn-Mg-Cu合金多孔骨支架免疫细胞形貌图与动物实验CT图。
具体实施方式
下面结合具体实施例对本发明作进一步说明。
实施例1
一种均匀降解的功能Zn-Mg-Cu合金多孔骨支架，其中Mg元素含量为3wt.％，Cu元素含量为2wt.％，余量为Zn元素。
本发明所述均匀降解的功能锌合金多孔骨支架的制备方法如下：
(1)按比例称取Zn粉、Cu粉和Mg粉，在氩气保护下进行球磨(球磨参数为250r/min，球磨时间为4h，同时在球磨过程中需要间歇1h)混合得到Zn-Mg-Cu合金粉末；其中，所述Zn粉、Cu粉和Mg粉均为球形，所述Zn粉和Mg粉粒径均为15-53μm；所述Cu粉粒径为10-30μm之间。
(2)将三维联通多孔结构(孔隙率67％)模型导入激光选区熔化设备，然后将Zn-Mg-Cu合金粉末进行打印，其中打印参数为：激光功率为100W，扫描速度为500mm/s，扫描策略为层间旋转67度，基板预热120℃，得到多孔支架
(3)将打印得到的多孔支架进行喷砂、超声处理，烘干后得到成品，其中超声处理是将多孔支架依次在去离子水、乙醇和丙酮中超声30min，直到无黑色金属粉末脱落。
微观组织观察表明，合金晶粒为等轴晶，平均尺寸在1.6μm，Mg和Cu元素可以均匀的分布在Zn基体当中，力学测试表明，Zn-Mg-Cu合金多孔支架抗压强度52MPa，弹性模量为2.0GPa，符合松质骨要求。
降解实验表明，降解产物在微宏观两个尺度均分布的均较为均匀(附图1和图2)，没有明显局部降解出现。
抗菌实验表明，Zn-Mg-Cu合金具有强于纯Zn的抗菌能力，形成的抑菌环直径更大(附图3)
免疫细胞培养实验表明，Zn-Mg-Cu合金表面的免疫细胞生长形态更好，密度更高，相对于纯Zn促进了免疫细胞的增殖。
兔股骨缺损动物实验表明，Zn-Mg-Cu合金多孔支架促进骨骼生长的能力远高于纯Zn多孔支架(附图4)，新骨生成体积更多。
实施例2
一种均匀降解的功能锌合金多孔骨支架为Zn-Mg-Fe合金，其中Mg元素含量为5wt.％，Fe元素含量为5wt.％，余量为Zn元素。
上述Zn-Mg-Fe合金，粉末制备按照实施例1的方法，加工参数为激光功率为100W，扫描速度为400mm/s。
实施例3
一种均匀降解的功能锌合金多孔骨支架为Zn-Mg-Ag合金，其中Mg元素含量为10wt.％，Ag元素含量为2wt.％，余量为Zn元素。
上述Zn-Mg-Fe合金，粉末制备按照实施例1的方法，加工参数为激光功率为150W，扫描速度为400mm/s。
对比例1
一种多孔骨支架，具体方法如下：
(1)以纯Zn粉为原材料，所述Zn粉为球形，所述Zn粉粒径为15-53μm。将三维联通多孔结构模型导入激光选区熔化设备，然后将Zn粉末进行打印，其中加工参数为：激光功率为80W，扫描速度为700mm/s，扫描策略为层间旋转67度，基板预热100℃，得到多孔支架。
(2)将打印得到的多孔支架进行喷砂、超声处理，烘干后得到成品，其中超声处理是将多孔支架依次在去离子水、乙醇和丙酮中超声30min，直到无黑色金属粉末脱落。
对比例2
一种多孔骨架，具体方法如下：
(1)按比例称取Zn粉和Mg粉(其中Mg元素含量为3wt.％)，在氩气保护下进行球磨(球磨参数为250r/min，球磨时间为4h，同时在球磨过程中需要间歇1h)混合得到Zn-Mg合金粉末；其中，所述Zn粉和Mg粉均为球形，所述Zn粉和Mg粉粒径均为15-53μm。
(2)将三维联通多孔结构模型导入激光选区熔化设备，然后将Zn-Mg合金粉末进行打印，其中中加工参数为：激光功率为90W，扫描速度为450mm/s，扫描策略为层间旋转67度，基板预热120℃，得到多孔支架
(3)将打印得到的多孔支架进行喷砂、超声处理，烘干后得到成品，其中超声处理是将多孔支架依次在去离子水、乙醇和丙酮中超声30min，直到无黑色金属粉末脱落。
从图3((A)为抑菌环形貌图，(B)为抑菌环半径统计图)和图4中可以看出，本发明加入的Mg元素，能够促进免疫细胞生长，提高细胞活性与增殖密度，通过免疫介导促进骨骼再生，Cu元素的加入有效增强了合金抗大肠杆菌和金葡萄球菌的能力。Mg和Cu元素协同为骨组织重建提供免疫介导成骨和抑菌抗感染的环境，同时促进多孔支架的均匀降解(图2)。
本发明所述多孔支架的降解均匀性和功能性能够在支架降解过程中持续保持，可有效加快植入体向健全骨组织的完全转化。解决了现有涂层技术无法在3D打印精细多孔支架表面良好制备的困境，以及涂层失效后无法在支架降解过程中提供功能性。
需要说明的是，以上列举的仅是本发明的若干个具体实施例，显然本发明不仅仅限于以上实施例，还可以有其他变形。本领域的技术人员从本发明公开内容直接导出或间接引申的所有变形，均应认为是本发明的保护范围。

Claims (4)

1.一种均匀降解的功能Zn合金多孔骨支架，其特征在于，所述多孔骨支架为Zn-Mg-X合金，其中Mg元素含量为3-20wt.％，X元素含量为1-5wt.％，余量为Zn元素；所述X元素为Cu、Fe或Ag中的一种；所述多孔骨支架中构建有X/Zn和Zn/Mg双重微电池；
所述均匀降解的功能锌合金多孔骨支架的制备方法，包括以下步骤：
(1)按比例称取Zn粉、X粉和Mg粉，在氩气保护下进行球磨混合得到Zn-Mg-X合金粉末；
(2)将三维联通多孔结构模型导入激光选区熔化设备，然后将Zn-Mg-X合金粉末进行打印，得到多孔支架；
(3)将打印得到的多孔支架进行喷砂、超声处理，烘干后得到成品；
步骤(2)所述激光选区熔化打印参数如下：
激光功率为60-150W，扫描速度为400-700mm/s，扫描策略为层间旋转67度，基板预热100-150℃。
2.根据权利要求1所述的均匀降解的功能Zn合金多孔骨支架，其特征在于，所述Zn粉、X粉和Mg粉均为球形，所述Zn粉和Mg粉粒径均为15-53μm；所述X粉粒径为10-30μm之间。
3.根据权利要求1所述的均匀降解的功能Zn合金多孔骨支架，其特征在于，步骤(1)所述的球磨参数为250r/min，球磨时间为4h，同时在球磨过程中需要间歇1h防止粉末粘黏。
4.根据权利要求1所述的均匀降解的功能Zn合金多孔骨支架，其特征在于，步骤(3)所述的超声处理是将多孔支架依次在去离子水、乙醇和丙酮中超声30min，直到无黑色金属粉末脱落。
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