CN109652768A - 一种医用植入材料用镁-锶涂层及其制备方法 - Google Patents
一种医用植入材料用镁-锶涂层及其制备方法 Download PDFInfo
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Abstract
为了提高现有骨植入材料的骨整合能力,本发明提供了一种医用植入材料用镁‑锶涂层及其制备方法,采用多弧离子镀技术,在钛、钛合金、不锈钢、高分子材料实体或多孔材料上制备金属镁‑锶涂层,该涂层的厚度为0.1‑200μm,涂层中锶元素的质量百分比为:0%<Sr≤10%。本发明能够解决现有植入材料组织相容性欠佳的问题,该方法所得涂层具极佳的生物相容性和骨生物活性。
Description
技术领域
本发明属于医用材料领域,特别涉及齿科植入物、关节置换和人体组织缺损的填充材料及植入材料抗菌技术领域;具体为在植入物表面涂覆的镁-锶涂层材料及其制备方法。
背景技术
由于植入假体松动和磨蚀引发的不良细胞反应使人工关节等植入体的骨整合能力差,只有10-15年的寿命,不能满足长期使用要求。金属材料一直以来被认为具有生物稳定性,虽然人们对其表面进行了各种表面改性的工作以提高金属材料的生物相容性及生物活性,但是骨细胞的粘附生长仍不理想。而金属镁(Mg),因为其具有较高的负电极电位,与水发生化学反应而降解,被人体吸收及代谢。同时,镁具有生物活性,可诱导细胞分化、生长和血管的长入,其作为植入器件植入生物体后,骨细胞向镁降解而减少的空间增殖、繁殖,随着镁逐步降解,形成新的具有原来特殊功能和形态的相应组织和器官,达到修复创伤和重建功能的目的。此外,由于镁降解而形成的碱性环境能达到抑制细菌生长的目的。镁由于其力学性能的限制只能用于非承力的部位,如手指、脚趾等。目前德国Syntellix公司制造的MAGNEZIX镁合金压缩螺钉通过了CE认证,韩国U&I公司制造的镁合金螺钉也通过了KFDA的批准,用于指关节的骨折固定。国内的中国科学院金属研究所等,正在与东莞宜安、江苏创生等医疗器械厂商进行镁合金产品申报。然而,上述产品均以实体块材形式应用,且用于非承力部位。目前未见将镁基材料以薄膜的形式复合于现有医用植入材料表面的相关报道,镁基材料以薄膜形式可应用于需承力部位,如人工关节等,这种新的使用形式将在医用植入材料领域发挥重要作用。金属锶(Sr)是人体骨中必须的元素之一,骨中锶含量约为骨质量的0.01%。在新骨形成初期,锶离子的浓度较高,随着骨基质的成熟,锶离子才逐渐被钙离子替代,锶元素能促进骨的形成,增加骨的强度,影响骨的再生能力,抑制骨吸收的同时刺激新骨的形成,因此锶对骨骼系统具有重要作用。
发明内容
为了提高现有骨植入材料的骨整合能力,本发明提供了一种医用植入材料用镁-锶涂层及其制备方法,采用多弧离子镀蒸镀技术,在钛、钛合金、不锈钢、高分子材料制备的实体及多孔结构基体表面制备镁-锶涂层,以解决现有植入材料组织相容性欠佳的问题,该方法所得涂层具极佳的生物相容性和骨生物活性。
本发明的技术方案如下:
一种医用植入材料用镁-锶涂层,其特征在于:镁-锶涂层的厚度为0.1-200μm,涂层中锶元素的质量百分比为:0%<Sr≤10%(优选3%<Sr≤6%)。
其中,所用基体为实体或多孔结构,采用钛、钛合金、不锈钢或高分子材料制成。所用实体基体优选为医用材料;所用多孔结构基体的孔隙率≧80%,孔径为200μm-5mm。
本发明所述材料特别适用于医用植入材料上,突破了镁基材料由于力学性能的不足而只能用于非承力部位的限制,将镁基材料涂覆于人工关节等材料表面,将镁基材料的应用领域拓展到需承力部位。
作为优选的技术方案,本发明所述涂层中还可引入金属银、锌及铜元素之一种或多种,其质量百分比为0%<Ag≤10%,0%<Zn≤3%,0%<Cu≤2%,以提高其抗菌性能。
本发明还提供了所述镁-锶涂层的制备方法,其特征在于:采用多弧离子镀技术将镁锶合金激发为离子,并沉积在基体表面形成涂层。
本发明所述述镁-锶涂层的制备方法,其特征在于:所述镁锶合金原料为熔化浇铸获得,镁原料为纯度≧99.99%纯镁块材,锶原料为纯度≧99.99%纯锶颗粒。
作为优选的工艺,偏压为40-120V,弧流为20-90A,占空比为20%-60%,工作气压为1×10-2-10Pa,轴向磁场为0-100mT。
本发明制备镁-锶涂层的具体步骤如下:
(1)、合金靶的制备:采用纯度为99.99%的镁和锶纯金属进行熔炼,得到合金锭,然后按照多弧离子镀设备所要求的靶材尺寸加工成阴极靶;
(2)、将基体依次用去离子水、无水乙醇超声清洗后,干燥氮气吹干送入沉积室;
(3)、抽极限真空至10-5Pa,后充入氩气,镀膜室真空度达到1.8×10-1-2.5×10- 1Pa,开启弧源,离子轰击清洗5-10分钟,然后在设定条件下进行涂层制备。
本发明的有益效果是:
1、本发明提出一种医用植入材料用镁-锶涂层,金属镁具有良好的生物相容性。镁与体液发生化学反应而降解,降解产物可随人体代谢排出体外。镁还具骨诱导、促血管化以及镁降解的碱性环境具有抗菌等多重生物功能性。金属锶能促进骨的形成,增加骨的强度,抑制骨吸收的同时刺激新骨的形成,对骨骼系统具有重要作用。在植入器件表面制备镁-锶涂层将发挥抗菌、促愈合及促组织生长的多重生物功能。
2、本发明提出的制备涂层的方法,可在多种骨科植入材料表面涂覆一定厚度的镁-锶涂层,适用于多种表面,不需要对材料表面进行特殊处理,适用范围广。
3、本发明解决了镁基材料只能用于非承力部位的问题,将镁基材料的应用领域扩展到承力部位,提升了镁基材料应用的可能性。
附图说明
图1为实施例1中沉积设备示意图。1、沉积室;2、供气系统;3、真空系统;4、靶材;5、基体;6、冷却系统。
具体实施方式
如图1所示,本发明方法所用的多弧离子镀设备的主体部分为沉积室,附属系统包括:真空系统、供电系统和供气系统。将沉积基体放在图中基体5的位置,将镁锶合金靶材放在靶材4的位置。在特定的真空条件及工作条件下,将镁锶合金靶材离子化,在电场及磁场的作用下,金属离子到达基体并沉积形成涂层。
实施例1
将钛合金(Ti-6Al-4V)原片置入沉积室炉体1中的基体5位置,将镁锶合金靶放在靶材4位置,Sr含量为1%,抽极限真空(10-5Pa)后,氩气反复清洗整个系统3次,以确保氧气含量降到最低。设定偏压为40V,弧流20A,占空比20%,工作气压为1×10-2Pa,沉积时间30min,沉积金属镁-锶层的厚度为1μm。为确定涂层的促成骨作用,进行了碱性磷酸酶(ALP)实验,培养1天,4天及7天后,涂层组颜色比基体组的更深,说明涂层组碱性磷酸酶的活性高于基体组,表明涂层具有促成骨作用。
实施例2
将多孔钛合金(Ti-6Al-4V)原片置入沉积室炉体1中的基体5位置,将镁锶合金靶放在靶材4位置,Sr含量为2%,抽极限真空(10-5Pa)后,氩气反复清洗整个系统3次,以确保氧气含量降到最低。设定偏压为50V,弧流30A,占空比30%,工作气压为1×10-2Pa,沉积时间1h,沉积金属镁-锶层的厚度为3μm。由于基体直接放置在基体托表面,因此与基体托接触的基体底部不能沉积涂层,可将基体翻转,将底部向上,再次沉积,将涂层完全覆盖于基体表面。也可使用金属丝将多孔基体悬挂起来,尽量减少多孔基体与工装的接触面积,这样单次即可将涂层完全覆盖于基体表面。
实施例3
将平面纯钛基体置入沉积室炉体1中的基体5位置,将镁锶合金靶放在靶材4位置,Sr含量为3%,抽极限真空(10-5Pa)后,氩气反复清洗整个系统3次,以确保氧气含量降到最低。设定偏压为55V,弧流45A,占空比40%,工作气压为1×10-1Pa,沉积时间1h,沉积金属镁-锶层的厚度为5μm。经过X射线衍射分析,以及扫描电镜能谱分析,确定涂层为镁锶,由于锶含量较少,X射线图谱仅可显示出金属镁的衍射信息。
实施例4
将平面316L不锈钢薄片置入沉积室炉体1中的基体5位置,将镁锶合金靶放在靶材4位置,Sr含量为4%,Cu含量为0.4%,抽极限真空(10-5Pa)后,氩气反复清洗整个系统3次,以确保氧气含量降到最低。设定偏压为65V,弧流60A,占空比40%,工作气压为1×10-1Pa,沉积时间1h,沉积金属镁-锶层的厚度为6μm。
实施例5
将平面高分子薄片置入沉积室炉体1中的基体5位置,将镁锶合金靶放在靶材4位置,Sr含量为5%,抽极限真空(10-5Pa)后,氩气反复清洗整个系统3次,以确保氧气含量降到最低。设定偏压为75V,弧流75A,占空比40%,工作气压为1Pa,沉积时间1h,沉积金属镁-锶层的厚度为8μm。
实施例6
将多孔钛合金(Ti-6Al-4V)样品置入沉积室炉体1中的基体5位置,将镁锶合金靶放在靶材4位置,Sr含量为7%,抽极限真空(10-5Pa)后,氩气反复清洗整个系统3次,以确保氧气含量降到最低。设定偏压为90V,弧流80A,占空比50%,工作气压为10Pa,沉积时间1h,沉积金属镁-锶层的厚度为9μm。
实施例7
将平面钛合金(Ti-6Al-4V)样品置入沉积室炉体1中的基体5位置,将镁锶合金靶放在靶材4位置,Sr含量为10%,抽极限真空(10-5Pa)后,氩气反复清洗整个系统3次,以确保氧气含量降到最低。设定偏压为120V,弧流90A,占空比60%,工作气压为10Pa,沉积时间1h,沉积金属镁-锶层的厚度为10μm。
实施例8
将平面钛合金(Ti-6Al-4V)样品置入沉积室炉体1中的基体5位置,将镁锶合金靶放在靶材4位置,Sr含量为8%,抽极限真空(10-5Pa)后,氩气反复清洗整个系统3次,以确保氧气含量降到最低。设定偏压为110V,弧流90A,占空比60%,工作气压为1Pa,沉积时间0.5h,轴向磁场95mT,沉积金属镁-锶层的厚度为190μm。
实施例9
将平面钛合金(Ti-6Al-4V)样品置入沉积室炉体1中的基体5位置,将镁锶合金靶放在靶材4位置,Sr含量为9%,抽极限真空(10-5Pa)后,氩气反复清洗整个系统3次,以确保氧气含量降到最低。设定偏压为120V,弧流90A,占空比60%,工作气压为10Pa,沉积时间2h,轴向磁场15mT,沉积金属镁-锶层的厚度为150μm。
将样品按照“JIS Z 2801-2000《抗菌加工制品-抗菌性试验方法和抗菌效果》、GB/T 2591-2003《抗菌塑料抗菌性能实验方法和抗菌效果》”等相关标准规定进行定量的抗菌性能检测。结果得到样品对常见感染菌(大肠杆菌、金黄色葡萄球菌)作用后的杀菌率为90%以上。
实施例结果表明,本发明采用多弧离子镀技术制备具有促成骨作用及抗菌作用的金属镁-锶涂层。将涂层制备于具有复杂几何外形的多孔材料、平面材料表面。采用该技术可提供镁-锶涂层的有效覆盖,可在提高医用材料骨长入能力的同时赋予材料抗菌性能。
实施例10
将平面钛合金(Ti-6Al-4V)样品置入沉积室炉体1中的基体5位置,将镁锶合金靶放在靶材4位置,Sr含量为8%,引入Ag含量为1%,Cu含量为0.1%,Zn含量为0.2%,抽极限真空(10-5Pa)后,氩气反复清洗整个系统3次,以确保氧气含量降到最低。设定偏压为100V,弧流80A,占空比50%,工作气压为1Pa,沉积时间1h,轴向磁场50mT,沉积金属镁-锶-银-铜-锌层的厚度为100μm。
将样品按照“JIS Z 2801-2000《抗菌加工制品-抗菌性试验方法和抗菌效果》、GB/T 2591-2003《抗菌塑料抗菌性能实验方法和抗菌效果》”等相关标准规定进行定量的抗菌性能检测。结果得到样品对常见感染菌(大肠杆菌、金黄色葡萄球菌)作用后的杀菌率为99%以上。其抗菌效果优于MgSr涂层。
上述实施例只为说明本发明的技术构思及特点,其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施,并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰,都应涵盖在本发明的保护范围之内。
Claims (10)
1.一种医用植入材料用镁-锶涂层,其特征在于:镁-锶涂层的厚度为0.1-200μm,涂层中锶元素的质量百分比为:0%<Sr≤10%。
2.按照权利要求1所述镁-锶涂层,其特征在于:涂层中锶元素的质量百分比为:3%<Sr≤6%。
3.按照权利要求1或2所述镁-锶涂层,其特征在于:所用基体为实体或多孔结构,采用钛、钛合金、不锈钢或高分子材料制成。
4.按照权利要求3所述镁-锶涂层,其特征在于:所用实体基体为医用材料;所用多孔结构基体的孔隙率≧80%,孔径为200μm-5mm。
5.按照权利要求1或2所述镁-锶涂层,其特征在于:所述涂层中引入金属银、锌及铜元素之一种或多种,其质量百分比为0%<Ag≤10%,0%<Zn≤3%,0%<Cu≤2%。
6.一种权利要求1所述述镁-锶涂层的制备方法,其特征在于:采用多弧离子镀技术制备涂层。
7.按照权利要求6所述述镁-锶涂层的制备方法,其特征在于:偏压为40-120V,弧流为20-90A,占空比为20%-60%。
8.按照权利要求6所述述镁-锶涂层的制备方法,其特征在于:工作气压为1×10-2-10Pa,轴向磁场为0-100mT。
9.按照权利要求6所述述镁-锶涂层的制备方法,其特征在于,具体制备步骤如下:
(1)、合金靶的制备:采用纯度为99.99%的镁和锶纯金属进行熔炼,得到合金锭,然后按照多弧离子镀设备所要求的靶材尺寸加工成阴极靶;
(2)、将基体依次用去离子水、无水乙醇超声清洗后,干燥氮气吹干送入沉积室;
(3)、抽极限真空至10-5Pa,后充入氩气,镀膜室真空度达到1.8×10-1-2.5×10-1Pa,开启弧源,离子轰击清洗5-10分钟,然后在设定条件下进行涂层制备。
10.一种权利要求1所述涂层在医用植入材料上的应用,其特征在于:所述医用植入材料为需承力部位所用植入物。
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