CN116196471A - 一种镁或镁合金表面负载兼具耐蚀性与抗菌性能的功能复合涂层及其制备方法、应用 - Google Patents
一种镁或镁合金表面负载兼具耐蚀性与抗菌性能的功能复合涂层及其制备方法、应用 Download PDFInfo
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Abstract
本发明提供在一种医用镁或镁合金表面负载耐蚀性且良好抗菌性能的功能复合涂层及其制备方法,属于金属材料表面处理技术领域。本发明所述方法包括:(一)将纯镁或镁合金为基体材料,将其浸入硝酸钆溶液,表面进行化学转化生成氧化钆涂层;(二)在氧化钆涂层表面采用浸涂法制备蜂胶/氧化石墨烯涂层。本发明通过在纯镁或镁合金表面制备该功能复合涂层,提高了基体的耐蚀性能、生物相容性及抗菌性,并提高了表面生物活性涂层蜂胶/氧化石墨烯与基体的结合强度,同时促进了医用镁或镁合金作为植入材料的成骨作用。
Description
技术领域
本发明属于医用镁和镁合金生物医用材料表面改性领域,具体涉及一种镁或镁合金表面负载兼具耐蚀性与抗菌性能的功能复合涂层及其制备方法、应用。
背景技术
生物镁或镁合金具有优良的力学相容性、承载能力、生物相容性、生物安全性和可降解特性。因此,生物镁或镁合金被认为是极具发展潜力的新型可降解生物医用材料,已经成为可降解生物医用材料的研发热点和前沿。然而,生物镁或镁合金材料的降解速率过快、生物相容性尚待提高是研究者共同关心的问题。
为解决生物镁或镁合金耐蚀性差及生物活性有待提高上述两大难题,研究者从合金化设计、生物镁及镁合金表面改性和塑性变形加工方面进行了一些研究工作。其中,表面改性是一种降低生物镁或镁合金腐蚀速率,控制其降解行为,也是提高表面生物相容性的最有效途径之一。与改变本体结构和成分相比,对生物镁或镁合金进行表面改性更简单、方便,表面改性一方面保持了材料良好本体属性,另一方面可调整表面的耐蚀性,使其降解可控;同时通过表面改性可以调整植入材料的硬度,赋予其抗菌、促进骨生长功能。
Cui等将氮气导入AZ31B(Mg-3Al-1Zn)镁合金中,发现其耐蚀性显著提高,但骨细胞相容性未见明显提高,并且其效果取决于注入电压和离子通量。且离子注入无法对合金提供长期保护,并且复杂器件存在注入困难的问题,因此有待进一步的探索。表面化学改性是通过化学或电化学反应在医用镁或镁合金表面形成新相。Cipriano等通过恒流阳极氧化在AZ31B 镁合金上形成了氧化镁膜,该膜层能有效延缓 AZ31B 镁合金的降解,但亦对成骨细胞增殖或新骨形成没有促进作用。而对生物镁或镁合金进行表面涂层改性的方法有很多,如等离子喷涂、电沉积、微弧氧化(MAO)、溶胶凝胶、静电纺丝等。目前,开展广泛研究的MAO涂层非常坚硬,有良好的耐磨性和耐腐蚀性、较好的热稳定性和介电性能。相关研究证实,随着制备电压的增加,MAO涂层的耐蚀性增强,但在高电压作用形成的陶瓷层的击穿孔也成为MAO涂层的缺陷。水热处理工艺简单,但涂层容易被破坏,而氟化处理过程使用强酸,存在一定危险性。通过不同的处理方法得到的涂层表面具有不同的粗糙度、孔隙率、力学性能以及生物学性能。
另外,蜂胶是较为常用的抗菌、消炎、调节免疫的药物,而且能促进组织的再生。J.H. Gao等先在Mg-Zn-Ca表面制备微弧氧化涂层,并在其表面制备蜂胶和聚乳酸复合涂层。并在复合涂层表面种植骨髓干细胞以观察其生长。但蜂胶的润湿性较差,作为基体涂层,不利于细胞的黏附和迁移。氧化石墨烯作为石墨烯的衍生物,具有亲水性能够增加其与相邻细胞以及细胞分泌物之间的接触,有研究显示,氧化石墨烯对血浆中的炎症细胞因子有较好的清除作用,而蜂胶与石墨烯的复合涂层国内外鲜有研究。
发明内容
基于此,本发明提供了一种镁或镁合金表面负载兼具耐蚀性与抗菌性能的功能复合涂层及其制备方法、应用,对医用镁或镁合金进行改性处理,在其表面上依次制备氧化钆中间过渡层、蜂胶与氧化石墨烯表层生物活性涂层,既提高医用镁或镁合金的耐腐蚀性,又增强其抗菌性和生物相容性等性能。
本发明的第一方面,提供一种镁或镁合金表面负载兼具耐蚀性与抗菌性能的功能复合涂层的制备方法,其中,所述制备方法包括如下步骤:
1)将医用镁或镁合金浸没入硝酸钆溶液中生成氧化钆转化涂层;
2)将步骤1)制备的表面覆盖有氧化钆涂层的医用镁或镁合金浸没到蜂胶与氧化石墨烯混合溶液中,恒速提拉取出,重复此操作多次,干燥,在医用镁或镁合金表面覆盖的氧化钆涂层上制得蜂胶/氧化石墨烯复合涂层。
进一步的,在步骤1)之前,对所述医用镁或镁合金表面进行抛光和干燥处理,所述医用镁或镁合金包括但不限于纯镁合金、Mg-Zn系合金、Mg-Al系合金,Mg-Ca系合金。
进一步的,步骤1)中将所述医用镁或镁合金浸入浓度为0.5%~1.5%的硝酸钆溶液中10~60min后,之后使用乙醇和去离子水交替冲洗、干燥,获得表面覆盖有氧化钆涂层的医用镁或镁合金。
进一步的,步骤2)中将表面覆盖有氧化钆膜的医用镁或镁合金垂直浸没到蜂胶与氧化石墨烯混合溶液中0.5~2h,以速度为1~3cm/min提拉取出,重复此操作多次,之后在50~80℃真空干燥2~12h,在医用镁或镁合金表面氧化钆涂层上制备厚度为2-5μm蜂胶/氧化石墨烯复合涂层。
进一步的,所述蜂胶与氧化石墨烯混合溶液制备方法包括如下步骤:
(1)将氧化石墨烯超声分散在N-甲基吡咯烷酮中;
(2)将步骤(1)得到的氧化石墨烯分散液进行过滤,获得粒径均匀的氧化石墨烯固体;
(3)将步骤(2)得到的氧化石墨烯烘干后重新超声分散在乙醇中,获得氧化石墨烯分散液;
(4)0.2g~20g的提纯蜂胶分别溶于50ml乙醇,磁力搅拌,静置,获得不同浓度的蜂胶分散液;
(5)将步骤(3)和(4)制备的氧化石墨烯分散液和蜂胶溶液按体积1~10/10比例进行混合,得到蜂胶与氧化石墨烯混合溶液。
进一步的,步骤(1)中氧化石墨烯在N-甲基吡咯烷酮超声分散1~2h,获得浓度为0.1~0.25mol/L氧化石墨烯分散液。
进一步的,步骤(3)中,将步骤(2)得到的氧化石墨烯烘干后重新超声分散在乙醇中,亦获得浓度为0.1~0.25mol/L氧化石墨烯酒精分散液。
进一步的,步骤(4)中提纯蜂胶溶于50ml乙醇中,磁力搅拌时间为1~2h。
本发明的第二方面,在镁或镁合金表面制得的兼具耐蚀性与抗菌性的功能复合涂层。
本发明的第三方面,表面负载兼具耐蚀性与抗菌性能的功能复合涂层的镁或镁合金作为制备植入材料的应用。
本发明提供的技术方案与现有技术相比具有如下优点:
(1)在医用镁或镁合金表面制备氧化钆化学转化中间涂层,以化学键与基体连接,增强了医用镁或镁合金基体耐蚀性,并且中间涂层表面呈现多孔微观结构,增大基体粗糙度,有利于提高蜂胶与氧化石墨烯复合涂层与基体表面的机械结合强度,有效降低了植入体服役过程中因结合强度较差造成涂层崩离及脱落现象;
(2)采用浸涂法在氧化钆中间涂层上覆盖蜂胶与氧化石墨烯复合涂层,蜂胶作为氧化石墨烯的载体,氧化石墨烯能增强蜂胶的润湿性,有利于增强细胞的黏附和迁移;
(3)在镁或镁合金表面上依次制备氧化钆涂层和蜂胶/氧化石墨烯复合涂层,有效延缓医用镁或镁合金基体表面和模拟体液的接触,电化学测试表明复合涂层的自腐蚀电位得到提高,自腐蚀电流密度得到降低,表明该功能复合涂层有效增强了医用镁或镁合金基体的耐蚀性;
(4)细胞实验中,采用DAPI对共培养一定时间后的氧化钆涂层表面负载蜂胶/氧化石墨烯复合涂层的镁合金表面的细胞进行染色,显示功能复合涂层表面的细胞要远多于镁合金基体表面的细胞,表明该复合涂层能有效增强医用镁或镁合金基体的生物活性及生物相容性,提高和优化了医用植入材料表面宿主细胞生长增殖状态;平板涂布法细菌实验还证明,该复合涂层能有效增强医用镁或镁合金基体的抗菌性能,避免了植入手术中因感染而造成的局部炎症的发生;
(5)本发明采用的化学转化及浸涂技术工艺简单易操作,制备复合涂层成本低。
附图说明
图1 本发明提供的功能复合涂层的制备示意图。
图2 Mg-Zn-Ca合金基体表面依次覆盖氧化钆涂层与蜂胶/氧化石墨烯复合涂层的XRD图(a),Mg-Zn-Ca合金基体表面氧化钆涂层的SEM图(b)、依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层的SEM图谱(c)。
图3 不同试样的极化曲线图:Mg-Zn-Ca基体(a);表面覆盖有氧化钆涂层的Mg-Zn-Ca基体(b);实施例1制得表面依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层的Mg-Zn-Ca基体(c)。
图4 Mg-Zn-Ca镁合金基体、及实例1制的的表面依次覆盖有氧化钆涂层、蜂胶与氧化石墨烯复合涂层采用MG63细胞共培养后,采用DAPI对共培养一定时间后的复合涂层表面的L929细胞进行染色情况。
(a) Mg-Zn-Ca基体,2h;(b) Mg-Zn-Ca基体,1d; (c) 表面覆盖有氧化钆涂层的Mg-Zn-Ca基体,2h; (d) 表面覆盖有氧化钆涂层的Mg-Zn-Ca基体,1d;(e) 表面依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层的Mg-Zn-Ca基体,2h;(f) 表面依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层的Mg-Zn-Ca基体,1d;标尺:200 μm。
图5 Mg-Zn-Ca基体、表面覆盖有氧化钆涂层的Mg-Zn-Ca基体,及实例1制得的表面依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层的平板涂布法细菌菌落:(a) Mg-Zn-Ca基体;(b) 表面覆盖有氧化钆涂层;(c) 表面依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层的功能医用材料。
具体实施方式
以下结合具体实施例对本发明的技术方案进行详细说明。以下实施例将有助于本领域的技术人员进一步理解本发明,但不以任何形式限制本发明。应当指出的是,对本领域的普通技术人员来说,在不脱离本发明的构思的前提下,还可以做出若干变形或改进。这行都属于本发明的保护范围。
下列实施例和性能测试中未注明具体的试验方法,通常按着常规条件进行。所选试剂或仪器未标明生产厂商者,均为可以通过市售购买获得的常规产品。
实施例1
一种在Mg-Zn-Ca基体表面依次制备氧化钆涂层与蜂胶/氧化石墨烯复合涂层的方法,包括如下步骤:
1)采用浇铸的方法制备Mg-Zn-Ca合金,制备过程详细可参考《Prepa-ration andcharacterization of a new biomedical Mg–Zn–Ca alloy》对制备的Mg-Zn-Ca合金进行打磨、抛光、干燥;
2)Mg-Zn-Ca合金浸入浓度为1%的硝酸钆(GdN3O9·6H2O,99.9%,aladdin)溶液中30min,在Mg-Zn-Ca合金表面生成氧化钆转化涂层;
3)将步骤2)制得的表面覆盖有氧化钆转化涂层的Mg-Zn-Ca合金使用无水乙醇和去离子水交替冲洗干净,自然风干;
4)将氧化石墨烯(C,10mg/ml, aladdin)加入到N-甲基吡咯烷酮(C5H9NO, 99.5%,aladdin)中,超声分散1h,配置成浓度为0.15mol/L氧化石墨烯分散液,然后过滤,烘干重新加入到乙醇中,超声2h,配置成浓度为0.15mol/L的氧化石墨烯分散液;将5g提纯蜂胶溶入50ml酒精中,磁力搅拌器搅拌1h,得到蜂胶分散液,将制备的氧化石墨烯分散液和蜂胶分散液按体积1/2比例进行混合,磁力搅拌器搅拌,得到蜂胶与氧化石墨烯混合溶液;
5)将表面覆盖有氧化钆中间层的Mg-Zn-Ca合金垂直浸入步骤4)制备的蜂胶与氧化石墨烯混合液中,浸没30min,之后以2cm/min将Mg-Zn-Ca合金试样从蜂胶与氧化石墨烯混合溶液中提拉取出,重复此项操作3次,Mg-Zn-Ca合金表面覆盖的蜂胶/氧化石墨烯复合涂层厚度为3μm,然后在80℃下真空干燥8h。
实施例2
一种在Mg-Zn-Y-Nd基体表面制备氧化钆涂层以及蜂胶与氧化石墨烯复合涂层的方法,包括如下步骤:
1)采用浇铸的方法制备Mg-Zn-Y-Nd合金,制备过程详细可参考
《Fabrication and characterization of biodegradable Mg-Zn-Y-Nd-Agalloy: Microstructure, mechanical properties, corrosion behavior andantibacterial activities》对制备的Mg-Zn-Y-Nd合金进行打磨、抛光、干燥;
2) Mg-Zn-Y-Nd合金浸入浓度为0.8%的硝酸钆(GdN3O9·6H2O,99.9%,aladdin)溶液中50min,在Mg-Zn-Y-Nd合金表面生成氧化钆转化膜层;
3)将步骤2)制得的表面覆盖有Mg-Zn-Y-Nd合金使用无水乙醇和去离子水交替冲洗干净,自然风干;
4) 将氧化石墨烯(C,10mg/ml, aladdin)加入到N-甲基吡咯烷酮(C5H9NO, 99.5%,aladdin)中,超声分散1.5h,配置成浓度为0.2mol/L氧化石墨烯分散液,然后过滤,烘干重新加入到乙醇中,超声1.5h,配置成浓度为0.2mol/L的氧化石墨烯分散液;将7.5g提纯蜂胶溶入50ml酒精中,磁力搅拌器搅拌1h,得到蜂胶分散液,将制备的氧化石墨烯分散液和蜂胶分散液按体积7/10比例进行混合,磁力搅拌器搅拌,得到蜂胶与氧化石墨烯混合液液;
5)将表面覆盖有氧化钆转化膜层的Mg-Zn-Y-Nd合金垂直浸入步骤4)制备的蜂胶与氧化石墨烯混合液中,浸没45min,之后以3cm/min将Mg-Zn-Ca合金试样从蜂胶与氧化石墨烯混合溶液中提拉取出,重复此项操作 5 次,待Mg-Zn-Ca合金覆盖的蜂胶与氧化石墨烯复合涂层厚度为 4μm,然后在70℃下真空干燥12h。
由于实施例2得到的复合涂层表征分析及性能测试与实施例1基本相同。因此,本发明具体实施过程中以实施例1为例对获得的表面依次覆盖有氧化钆涂层、蜂胶与氧化石墨烯复合涂层的Mg-Zn-Ca基体进行表征分析及性能测试。
以实施例1为例进行复合涂层表征分析及性能测试
图1 为本发明提供的医用材料功能复合涂层的制备示意图。
图2为Mg-Zn-Ca合金基体表面依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层的SEM图谱和XRD图谱,由(a)可知,复合涂层的XRD图谱中出现氧化钆、石墨烯、α-Mg衍射峰,由(b) 可知,氧化钆涂层呈多孔结构,蜂胶/氧化石墨烯复合涂层均匀附着在氧化钆涂层上,并无明显纤维裂纹(c)。
图3为不同试样的极化曲线图:Mg-Zn-Ca基体(a);表面覆盖有氧化钆涂层的Mg-Zn-Ca基体(b);实施例1制得表面依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层的Mg-Zn-Ca基体(c),测试其耐腐蚀性能,表面依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层的电位(potential,V)高于覆盖有氧化钆涂层的Mg-Zn-Ca基体和单一Mg-Zn-Ca基体,可见,该功能复合涂层提高了基体材料的耐腐蚀性能。
图4 Mg-Zn-Ca基体、及实例1制得的表面依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层的Mg-Zn-Ca基体采用MG63细胞共培养后,采用DAPI对共培养一定时间后的涂层表面的L929细胞进行染色情况;
(a) Mg-Zn-Ca基体,2h;(b) Mg-Zn-Ca基体,1d; (c) 表面覆盖有氧化钆涂层的Mg-Zn-Ca基体,2h; (d) 表面覆盖有氧化钆涂层的Mg-Zn-Ca基体,1d;(e) 表面依次覆盖有氧化钆涂层、蜂胶/氧化石墨烯复合涂层的Mg-Zn-Ca基体,2h;(f) 表面依次覆盖有氧化钆涂层、蜂胶/氧化石墨烯复合涂层的Mg-Zn-Ca基体,1d。由图4可知,我们采用DAPI(DAPI是一种可以穿透细胞膜的蓝色荧光染料)对共培养一定时间后的复合涂层表面的细胞进行染色,我们发现,在共培养2h、1d时,表面依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层表面的细胞要比Mg-Zn-Ca基体表面及氧化钆转化涂层表面的细胞多,说明表面依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层的基体表面细胞的生长增殖状态好,因为在细胞实验中,宿主的细胞与骨植入材料之间的相互作用,主要受材料的理化性质如化学组成、微观形貌或表面能等影响。材料的这些理化性能直接会影响到细胞的生物学行为-粘附、增殖和分化。而氧化钆涂层与蜂胶/氧化石墨烯涂层形成的功能复合涂层有助于提高医用植入材料表面宿主细胞生长增殖状态。
图5 不同试样采用平板涂布接种法抗菌实验图:(a) Mg-Zn-Ca基体;(b) 表面覆盖有氧化钆涂层;(c) 表面依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层。与图(a)和(b)相比,图(c)中没有细菌株,表明该功能复合涂层明显提高了试样的抗菌能力。相较于(a)Mg-Zn-Ca基体而言,表面覆盖有氧化钆涂层(b)的表面琼脂上反而产生比镁合金基体还要多的菌株,主要是由于氧化钆涂层一定程度上增强了试样的耐蚀性,反而降低了因镁基体腐蚀导致的琼脂较高的pH值,而涂层本身并无抑菌成分,反而更利于细菌的增殖。
表1为不同试样的电化学腐蚀参数。由表1可知,引入了氧化钆层与蜂胶/氧化石墨烯复合层形成的功能复合涂层后,电化学测试表明,相较于单一的氧化钆涂层,表面依次覆盖有氧化钆涂层与蜂胶/氧化石墨烯复合涂层的Mg-Zn-Ca基体的腐蚀电位有所提高,腐蚀电流降低了2个数量级,而且与单一Mg-Zn-Ca基体相比,腐蚀电流还降低了近3个数量级,能大大提高医用镁或镁合金的耐腐蚀性能。
Claims (10)
1.一种镁或镁合金表面负载兼具耐蚀性与抗菌性能的功能复合涂层的制备方法,其特征在于,所述制备方法包括如下步骤:
将医用镁或镁合金浸没入硝酸钆溶液中生成氧化钆转化涂层;
将步骤1)制备的表面覆盖有氧化钆涂层的医用镁或镁合金浸没到蜂胶与氧化石墨烯混合溶液中,恒速提拉取出,重复此操作多次,干燥,在医用镁或镁合金表面经化学转化制成的氧化钆涂层上浸涂得到蜂胶/氧化石墨烯复合涂层。
2.根据权利要求1所述的镁或镁合金表面负载兼具耐蚀性与抗菌性能的功能复合涂层的制备方法,其特征在于,在步骤1)之前,对所述医用镁或镁合金表面进行抛光和干燥处理,所述镁或镁合金包括但不限于纯镁合金、Mg-Zn系合金、Mg-Al系合金,Mg-Ca系合金。
3.根据权利要求1所述的镁或镁合金表面负载兼具耐蚀性与抗菌性能的功能复合涂层的制备方法,其特征在于,步骤1)中将所述医用镁合金浸入浓度为0.5%~1.5%的硝酸钆溶液中10~60min后,之后使用乙醇和去离子水交替冲洗、干燥,在医用镁或镁合金表面覆盖有氧化钆涂层。
4.根据权利要求1所述的镁或镁合金表面负载兼具耐蚀性与抗菌性能的功能复合涂层的制备方法,其特征在于,步骤2)中将表面覆盖有氧化钆膜的医用镁或镁合金垂直浸没到蜂胶与氧化石墨烯混合溶液中0.5~2h,以速度为1~3cm/min提拉取出,重复此操作多次,之后在50~80℃真空干燥2~12h,在医用镁或镁合金表面氧化钆涂层上制备厚度为2-5μm蜂胶/氧化石墨烯复合涂层。
5.根据权利要求1或4所述的镁或镁合金表面负载兼具耐蚀性与抗菌性能的功能复合涂层的制备方法,其特征在于,所述蜂胶与氧化石墨烯混合溶液制备方法包括如下步骤:
(1)将氧化石墨烯超声分散在N-甲基吡咯烷酮中;
(2)将步骤(1)得到的氧化石墨烯分散液进行过滤,获得粒径均匀的氧化石墨烯固体;
(3)将步骤(2)得到的氧化石墨烯烘干后重新超声分散在乙醇中,获得氧化石墨烯分散液;
(4)0.2g~20g的提纯蜂胶分别溶于50ml乙醇,磁力搅拌,静置,获得不同浓度的蜂胶分散液;
(5)将步骤(3)和(4)制备的氧化石墨烯分散液和蜂胶溶液按体积1~10/10比例进行混合,得到蜂胶与氧化石墨烯混合溶液。
6.根据权利要求5所述的镁或镁合金表面负载兼具耐蚀性与抗菌性能的功能复合涂层的制备方法,其特征在于,步骤(1)中氧化石墨烯在N-甲基吡咯烷酮超声分散1~2h,获得浓度为0.1~0.25mol/L氧化石墨烯分散液。
7.根据权利要求5所述的镁或镁合金表面负载兼具耐蚀性与抗菌性能的功能复合涂层的制备方法,其特征在于,步骤(3)中,将步骤(2)得到的氧化石墨烯烘干后重新超声分散在乙醇中,获得浓度为0.1~0.25mol/L氧化石墨烯酒精分散液。
8.根据权利要求5所述的镁或镁合金表面负载兼具耐蚀性与抗菌性能的功能复合涂层的制备方法,其特征在于,步骤(4)中提纯蜂胶溶于50ml乙醇中,磁力搅拌时间为1~2h。
9.权利要求1至8任一项所述的制备方法在镁或镁合金表面制得的兼具耐蚀性与抗菌性的功能复合涂层。
10.权利要求9所述的表面负载兼具耐蚀性与抗菌性能的功能复合涂层的镁或镁合金作为制备植入材料的应用。
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