CN113230453A - 一种医用镁合金耐腐蚀涂层的制备方法 - Google Patents
一种医用镁合金耐腐蚀涂层的制备方法 Download PDFInfo
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Abstract
本发明公开了一种医用镁合金耐腐蚀涂层的制备方法,包括镁合金基体预处理:将镁合金使用800~1000目砂纸进行打磨,然后放置在蒸馏水超声洗涤45~60min后吹干;将明胶和脱乙酰壳聚糖加入到乙酸溶液中,超声搅拌并加入纳米羟基磷灰石,在室温条件下持续搅拌12~16h使其充分溶胀,然后将步骤S1中预处理后的镁合金置于磁控溅射镀膜装置中,进行磁控溅射镀膜;将步骤S2中的有涂层的镁合金置于氮气条件下,并升温至120~130℃保温3~4h后冷却,再次置于磁控溅射装置中,以步骤S2中相同条件进行磁控溅射镀膜,只改变溅射时间为0.5~1.5h;将步骤S3中得到的涂层合金置于真空环境下,室温放置24~48h,然后再次置于氮气环境下加热至135~140℃保温1~2h,冷却得到所述耐腐蚀涂层的镁合金。
Description
技术领域
本发明属于镁合金防腐蚀技术领域,具体涉及一种医用镁合金耐腐蚀涂层的制备方法。
背景技术
可植入生物医用金属材料凭借着优良的机械性能、抗压强度和耐腐蚀性能,成为了最早植入生物体的医用材料,其在医学上得到了广泛应用,包括人工关节、心脏起搏器、心血管、肾瓣膜和牙齿等。其中,镁合金表现出与人体骨骼较为接近的力学性能,在人体中可以弱化骨骼和植入物之间的负载转移,减少应力屏蔽效应。
然而,单纯的医用镁合金材料在植入人体一段时间之后会与人体组织发生反应,使得镁合金材料因腐蚀速率过快难以完成其功能,所以通常在镁合金材料表面涂覆一层具有生物活性的涂层,如羟基磷灰石。这样,既能提高其耐腐性性能,又能增强其在临床医学的应用范围。传统的金属植入物如:不锈钢和钛合金等,存在着弹性模量与天然骨骼的差异较大,容易引起应力屏蔽,不利于新骨生长;同时,在帮助受损组织修复之后需通过二次手术将植入物移除。为了再次手术一出植入物,逐渐使用可降解的骨科植入物,如用作关节固定的镁合金骨钉在植入后的18个月后可完全降解,因此不需再次手术将其取出,具有良好的便利性。
发明内容
针对现有技术中羟基磷灰石作为涂层时,该涂层较为脆弱,镁合金产生氢气致使涂层溶胀进而使涂层的防腐蚀效果变差,本发明的目的是提供一种医用镁合金耐腐蚀涂层的制备方法,所述制备方法包括以下步骤:
S1:镁合金基体预处理:将镁合金使用800~1000目砂纸进行打磨,然后放置在蒸馏水超声洗涤45~60min后吹干,备下步使用。
S2:将明胶和脱乙酰壳聚糖加入到乙酸溶液中,超声搅拌并加入纳米羟基磷灰石,在室温条件下持续搅拌12~16h使其充分溶胀,然后将步骤S1中预处理后的镁合金置于磁控溅射镀膜装置中,进行磁控溅射镀膜。
S3:将步骤S2中的有涂层的镁合金置于氮气条件下,并升温至120~130℃保温3~4h后冷却,再次置于磁控溅射装置中,以步骤S2中相同条件进行磁控溅射镀膜,只改变溅射时间为0.5~1.5h。
S4:将步骤S3中得到的涂层合金置于真空环境下,室温放置24~48h,然后再次置于氮气环境下加热至135~140℃保温1~2h,冷却得到所述耐腐蚀涂层的镁合金。
作为优选方案,上述所述的镁合金为ZK61镁合金、AZ61A镁合金、AZ91D镁合金和AZ31B镁合金中的任意一种。
作为优选方案,上述所述的明胶、脱乙酰壳聚糖和乙酸的质量体积比为(0.75~1.5)g:(1.05~1.58)g:(15~25)mL。
作为优选方案,上述所述的纳米羟基磷灰石和脱乙酰壳聚糖的质量比为(1~2):(0.45~0.69)。
作为优选方案,上述所述的磁控溅射镀膜的靶材-基体间距为42~45mm,本地真空度为5.5~6Pa,溅射功率为360~390W,溅射时间为3~5h。
与现有技术相比,本发明具有如下有益效果:
本发明中,采用明胶和脱乙酰壳聚糖再与羟基磷灰石在乙酸溶液中静置溶胀采用磁控溅射技术镀膜、加热处理、二次镀膜、加热处理后得到的耐腐蚀涂层具有较优异的防腐蚀效果,在模拟体液中800h以后发生腐蚀效果,同时本发明涂层还具有较优异的柔韧性,对涂层不进行低温冷冻处理,能够有效的降低羟基磷灰石涂层的脆性,进而进一步提高涂层的防腐蚀性能。
附图说明
图1为本发明实施例1和对比例1涂层在水热条件下20天后的SEM图谱。
具体实施方式
下面对本发明实施例作具体详细的说明,本实施例在本发明技术方案为前提下进行实施,给出了详细的实施方式和具体的操作过程,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
实施例1
一种医用镁合金耐腐蚀涂层的制备方法,具体包括以下步骤:
S1:镁合金基体预处理:将ZK61镁合金使用800目砂纸进行打磨,然后放置在蒸馏水超声洗涤45min后吹干,备下步使用。
S2:将明胶和脱乙酰壳聚糖加入到乙酸溶液中,超声搅拌并加入纳米羟基磷灰石,在室温条件下持续搅拌12h使其充分溶胀,然后将步骤S1中预处理后的镁合金置于磁控溅射镀膜装置中,进行磁控溅射镀膜;其中明胶、脱乙酰壳聚糖和乙酸的质量体积比为0.75g:1.05g:15mL;纳米羟基磷灰石和脱乙酰壳聚糖的质量比为1:0.45;磁控溅射镀膜的靶材-基体间距为42mm,本地真空度为5.5Pa,溅射功率为360W,溅射时间为3h。
S3:将步骤S2中的有涂层的镁合金置于氮气条件下,并升温至120℃保温3h后冷却,再次置于磁控溅射装置中,以步骤S2中相同条件进行磁控溅射镀膜,只改变溅射时间为0.5h。
S4:将步骤S3中得到的涂层合金置于真空环境下,室温放置24h,然后再次置于氮气环境下加热至135℃保温1h,冷却得到所述耐腐蚀涂层的镁合金。
实施例2
一种医用镁合金耐腐蚀涂层的制备方法,具体包括以下步骤:
S1:镁合金基体预处理:将AZ61A镁合金使用1000目砂纸进行打磨,然后放置在蒸馏水超声洗涤60min后吹干,备下步使用。
S2:将明胶和脱乙酰壳聚糖加入到乙酸溶液中,超声搅拌并加入纳米羟基磷灰石,在室温条件下持续搅拌16h使其充分溶胀,然后将步骤S1中预处理后的镁合金置于磁控溅射镀膜装置中,进行磁控溅射镀膜;其中明胶、脱乙酰壳聚糖和乙酸的质量体积比为1.5g:1.58g:25mL;纳米羟基磷灰石和脱乙酰壳聚糖的质量比为2:0.69;磁控溅射镀膜的靶材-基体间距为45mm,本地真空度为6Pa,溅射功率为390W,溅射时间为5h。
S3:将步骤S2中的有涂层的镁合金置于氮气条件下,并升温至130℃保温4h后冷却,再次置于磁控溅射装置中,以步骤S2中相同条件进行磁控溅射镀膜,只改变溅射时间为1.5h。
S4:将步骤S3中得到的涂层合金置于真空环境下,室温放置48h,然后再次置于氮气环境下加热至140℃保温2h,冷却得到所述耐腐蚀涂层的镁合金。
实施例3
一种医用镁合金耐腐蚀涂层的制备方法,具体包括以下步骤:
S1:镁合金基体预处理:将AZ91D镁合金使用900目砂纸进行打磨,然后放置在蒸馏水超声洗涤50min后吹干,备下步使用。
S2:将明胶和脱乙酰壳聚糖加入到乙酸溶液中,超声搅拌并加入纳米羟基磷灰石,在室温条件下持续搅拌14h使其充分溶胀,然后将步骤S1中预处理后的镁合金置于磁控溅射镀膜装置中,进行磁控溅射镀膜;其中明胶、脱乙酰壳聚糖和乙酸的质量体积比为0.96g:1.24g:20mL;纳米羟基磷灰石和脱乙酰壳聚糖的质量比为1.3:0.52;磁控溅射镀膜的靶材-基体间距为43mm,本地真空度为5.7Pa,溅射功率为370W,溅射时间为4h。
S3:将步骤S2中的有涂层的镁合金置于氮气条件下,并升温至125℃保温3.5h后冷却,再次置于磁控溅射装置中,以步骤S2中相同条件进行磁控溅射镀膜,只改变溅射时间为1h。
S4:将步骤S3中得到的涂层合金置于真空环境下,室温放置35h,然后再次置于氮气环境下加热至137℃保温1.5h,冷却得到所述耐腐蚀涂层的镁合金。
实施例4
一种医用镁合金耐腐蚀涂层的制备方法,具体包括以下步骤:
S1:镁合金基体预处理:将AZ31B镁合金使用950目砂纸进行打磨,然后放置在蒸馏水超声洗涤55min后吹干,备下步使用。
S2:将明胶和脱乙酰壳聚糖加入到乙酸溶液中,超声搅拌并加入纳米羟基磷灰石,在室温条件下持续搅拌15h使其充分溶胀,然后将步骤S1中预处理后的镁合金置于磁控溅射镀膜装置中,进行磁控溅射镀膜;其中明胶、脱乙酰壳聚糖和乙酸的质量体积比为1.4g:1.52g:24mL;纳米羟基磷灰石和脱乙酰壳聚糖的质量比为1.6:0.65;磁控溅射镀膜的靶材-基体间距为44mm,本地真空度为5.8Pa,溅射功率为380W,溅射时间为4h。
S3:将步骤S2中的有涂层的镁合金置于氮气条件下,并升温至128℃保温3h后冷却,再次置于磁控溅射装置中,以步骤S2中相同条件进行磁控溅射镀膜,只改变溅射时间为1.2h。
S4:将步骤S3中得到的涂层合金置于真空环境下,室温放置45h,然后再次置于氮气环境下加热至139℃保温1h,冷却得到所述耐腐蚀涂层的镁合金。
对比例1
根据CN 112391600 A中实施例1所描述的方法得到。
性能测试:为了验证本发明的耐腐蚀性能,对上述实施例1-4和对比例1做浸泡实验,在模拟体液(SBF)中,37℃下对镁合金长期保护能力的测试。将实施例1~4和对比例1中包含涂层的镁合金片和裸露的镁合金片进行封装,防止边缘效应,而后将其各自置于盛有模拟液的烧杯中,用保鲜膜封住烧杯口,放入37℃的恒温水浴锅中,每两天更新一次模拟体液,并记录样品开始发生腐蚀的情况,测试结果如表1所示,时间表示样品开始发生腐蚀的时间;
表1.测试结果:
从表1中可以看出,本发明实施例1~4制备的耐腐蚀涂层发生腐蚀的时间均在800h以上,相比较对比例1中的有涂层的镁合金的腐蚀时间623h具有良好的耐腐蚀效果,同时在对实施例1和对比例1在水热条件下放置20天以后,表征其涂层的SEM(图1)可以得知,实施例1中的涂层表面依然光滑没有裂纹,而对比例1中涂层表面有裂纹,说明本发明涂层具有良好的柔韧性而对比例1中的涂层依然有较高的脆性。
Claims (5)
1.一种医用镁合金耐腐蚀涂层的制备方法,其特征在于,所述制备方法包括以下步骤:
S1:镁合金基体预处理:将镁合金使用800~1000目砂纸进行打磨,然后放置在蒸馏水超声洗涤45~60min后吹干,备下步使用;
S2:将明胶和脱乙酰壳聚糖加入到乙酸溶液中,超声搅拌并加入纳米羟基磷灰石,在室温条件下持续搅拌12~16h使其充分溶胀,然后将步骤S1中预处理后的镁合金置于磁控溅射镀膜装置中,进行磁控溅射镀膜;
S3:将步骤S2中的有涂层的镁合金置于氮气条件下,并升温至120~130℃保温3~4h后冷却,再次置于磁控溅射装置中,以步骤S2中相同条件进行磁控溅射镀膜,只改变溅射时间为0.5~1.5h;
S4:将步骤S3中得到的涂层合金置于真空环境下,室温放置24~48h,然后再次置于氮气环境下加热至135~140℃保温1~2h,冷却得到所述耐腐蚀涂层的镁合金。
2.根据权利要求1所述的一种医用镁合金耐腐蚀涂层的制备方法,其特征在于,所述的镁合金为ZK61镁合金、AZ61A镁合金、AZ91D镁合金和AZ31B镁合金中的任意一种。
3.根据权利要求1所述的一种医用镁合金耐腐蚀涂层的制备方法,其特征在于,所述的明胶、脱乙酰壳聚糖和乙酸的质量体积比为(0.75~1.5)g:(1.05~1.58)g:(15~25)mL。
4.根据权利要求1所述的一种医用镁合金耐腐蚀涂层的制备方法,其特征在于,所述的纳米羟基磷灰石和脱乙酰壳聚糖的质量比为(1~2):(0.45~0.69)。
5.根据权利要求1所述的一种医用镁合金耐腐蚀涂层的制备方法,其特征在于,所述的磁控溅射镀膜的靶材-基体间距为42~45mm,本地真空度为5.5~6Pa,溅射功率为360~390W,溅射时间为3~5h。
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