CN112501570A - 一种金属/dlc复合薄膜及其制备方法 - Google Patents
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Abstract
本发明提供一种金属/DLC复合薄膜及其制备方法,采用磁控溅射法在医用镁合金表面制备金属/DLC复合薄膜,将金属Ag和/或Cu掺入制备DLC薄膜的石墨靶材中,克服了传统DLC薄膜容易粘附细菌的问题,使得镁合金DLC薄膜能够适用于对抗菌性能有一定要求的医疗场景。
Description
技术领域
本发明涉及医用材料复合薄膜领域,具体涉及一种金属/DLC复合薄膜及其制备方法。
背景技术
全关节置换术被认为是生物材料和生物工程领域最伟大的成就之一。人造关节在使用过程中产生的大量摩擦颗粒会进入关节周围组织中,导致骨溶解和假体松动。类金刚石(DLC)薄膜具有硬度高、表面光滑、摩擦系数小、耐磨损和耐腐蚀的特点。更重要的是,DLC具有人体组织相容性和血液相容性,对人体无副作用。由于上述优点,DLC薄膜被广泛应用于人体关节的医用材料领域。
虽然DLC薄膜具有诸多优点,但是DLC薄膜本身不具备抗菌作用,导致其表面容易粘附细菌,进而使其在对抗菌性能有一定要求的医疗场合无法使用。因此,如何使得医用DLC薄膜具备抗菌性能成为了急需解决的技术问题。
发明内容
针对现有技术存在的问题,本发明的目的在于提供一种金属/DLC复合薄膜及其制备方法,通过向DLC薄膜中掺入具有抗菌作用的金属粒子,使得薄膜材料具有优异的抗菌效果,拓宽了DLC薄膜的医疗应用领域。
一种镁合金表面的金属/DLC复合薄膜,所述金属/DLC复合薄膜由磁控溅射法制备而得,其特征在于:所述磁控溅射法选用金属/石墨复合靶材,其中金属含量为3.8 at.%-9.8 at.%,余量为石墨;所述金属选自Ag和Cu中的一种或多种。
优选地,所述金属为Ag和Cu。
优选地,所述复合靶材中金属Ag的含量为6 at.%,金属铜的含量为3.8 at.%。
进一步地,本发明还提供了一种镁合金表面的金属/DLC复合薄膜的制备方法,其特征在于:包括如下步骤:
A.选用镁合金为基体材料,将其切割为20×20×5mm;
B.依次用无水乙醇、去离子水超声清洗镁合金基体5min,然后烘干待用;
C.选用金属/石墨复合靶材,对复合靶材进行反溅射以清除表面的氧化物杂质;
D.将镁合金放入磁控溅射镀膜机中,抽真空使本底真空度低于5Pa,通入氩气为工作气体,开启溅射电源,对镁合金基体进行磁控溅射,其中,靶基距为50mm,溅射功率为380W,溅射时间为60min,溅射温度为120℃,氩气流量为120sccm。
优选地,所述金属含量为3.8 at.%-9.8 at.%,余量为石墨;所述金属选自Ag和Cu中的一种或多种。
优选地,所述金属为Ag和Cu。
优选地,所述复合靶材中金属Ag的含量为6 at.%,金属铜的含量为3.8 at.%。
优选地,所述镁合金为医用镁合金。
本发明采用磁控溅射法在医用镁合金表面制备金属/DLC复合薄膜,将金属Ag和/或Cu掺入制备DLC薄膜的石墨靶材中,克服了传统DLC薄膜容易粘附细菌的问题,使得镁合金DLC薄膜能够适用于对抗菌性能有一定要求的医疗场景。
另外,发明人意外地发现特定的金属粒子掺入量(6.0at.%Ag/3.8at.%Cu)可以将金属/DLC复合薄膜的抗菌率提高到98%以上,也就是说,在特定配比下两种抗菌粒子发生了协同作用,使得抗菌性能获得了惊人地提升。这一发现使得镁合金表面的金属/DLC复合薄膜可以应用于对抗菌性能要求极高的医疗领域。
具体实施方式
以下通过具体实施例来阐述本发明的技术方案,但是本发明的技术方案不仅局限于此。
实施例1
一种金属/DLC复合薄膜的制备方法,包括以下步骤:
A. 选用镁合金为基体材料,将其切割为20×20×5mm;
B. 依次用无水乙醇、去离子水超声清洗镁合金基体5min,然后烘干待用;
C. 选用Ag/石墨复合靶材(其中金属银的含量为6at.%),对复合靶材进行反溅射以清除表面的氧化物杂质;
D. 将镁合金放入磁控溅射镀膜机中,抽真空使本底真空度低于5Pa,通入氩气为工作气体,开启溅射电源,对镁合金基体进行磁控溅射,其中靶基距为50mm,溅射功率为380W,溅射时间为60min,溅射温度为120℃,氩气流量为120sccm;
E. 对表面镀覆有Ag/DLC复合薄膜的镁合金材料进行热处理,以消除薄膜应力。
实施例2
一种金属/DLC复合薄膜的制备方法,包括以下步骤:
A.选用镁合金为基体材料,将其切割为20×20×5mm;
B.依次用无水乙醇、去离子水超声清洗镁合金基体5min,然后烘干待用;
C.选用Cu/石墨复合靶材(其中金属铜的含量为6at.%),对复合靶材进行反溅射以清除表面的氧化物杂质;
D.将镁合金放入磁控溅射镀膜机中,抽真空使本底真空度低于5Pa,通入氩气为工作气体,开启溅射电源,对镁合金基体进行磁控溅射,其中靶基距为50mm,溅射功率为380W,溅射时间为60min,溅射温度为120℃,氩气流量为120sccm;
E.对表面镀覆有Cu/DLC复合薄膜的镁合金材料进行热处理,以消除薄膜应力。
实施例3
一种金属/DLC复合薄膜的制备方法,包括以下步骤:
A.选用镁合金为基体材料,将其切割为20×20×5mm;
B.依次用无水乙醇、去离子水超声清洗镁合金基体5min,然后烘干待用;
C.选用Cu/石墨复合靶材(其中金属铜的含量为3.8at.%),对复合靶材进行反溅射以清除表面的氧化物杂质;
D.将镁合金放入磁控溅射镀膜机中,抽真空使本底真空度低于5Pa,通入氩气为工作气体,开启溅射电源,对镁合金基体进行磁控溅射,其中靶基距为50mm,溅射功率为380W,溅射时间为60min,溅射温度为120℃,氩气流量为120sccm;
E.对表面镀覆有Cu/DLC复合薄膜的镁合金材料进行热处理,以消除薄膜应力。
实施例4
一种金属/DLC复合薄膜的制备方法,包括以下步骤:
A.选用镁合金为基体材料,将其切割为20×20×5mm;
B.依次用无水乙醇、去离子水超声清洗镁合金基体5min,然后烘干待用;
C.选用Ag/石墨复合靶材(其中金属银的含量为3.8at.%),对复合靶材进行反溅射以清除表面的氧化物杂质;
D.将镁合金放入磁控溅射镀膜机中,抽真空使本底真空度低于5Pa,通入氩气为工作气体,开启溅射电源,对镁合金基体进行磁控溅射,其中靶基距为50mm,溅射功率为380W,溅射时间为60min,溅射温度为120℃,氩气流量为120sccm;
E.对表面镀覆有Ag/DLC复合薄膜的镁合金材料进行热处理,以消除薄膜应力。
实施例5
一种金属/DLC复合薄膜的制备方法,包括以下步骤:
A.选用镁合金为基体材料,将其切割为20×20×5mm;
B.依次用无水乙醇、去离子水超声清洗镁合金基体5min,然后烘干待用;
C.选用Cu/Ag/石墨复合靶材(其中金属银的含量为6.0at.%,金属铜的含量为3.8at.%),对复合靶材进行反溅射以清除表面的氧化物杂质;
D.将镁合金放入磁控溅射镀膜机中,抽真空使本底真空度低于5Pa,通入氩气为工作气体,开启溅射电源,对镁合金基体进行磁控溅射,其中靶基距为50mm,溅射功率为380W,溅射时间为60min,溅射温度为120℃,氩气流量为120sccm;
E.对表面镀覆有Cu/Ag/DLC复合薄膜的镁合金材料进行热处理,以消除薄膜应力。
实施例6
一种金属/DLC复合薄膜的制备方法,包括以下步骤:
A.选用镁合金为基体材料,将其切割为20×20×5mm;
B.依次用无水乙醇、去离子水超声清洗镁合金基体5min,然后烘干待用;
C.选用Ag/石墨复合靶材(其中金属银的含量为9.8at.%),对复合靶材进行反溅射以清除表面的氧化物杂质;
D.将镁合金放入磁控溅射镀膜机中,抽真空使本底真空度低于5Pa,通入氩气为工作气体,开启溅射电源,对镁合金基体进行磁控溅射,其中靶基距为50mm,溅射功率为380W,溅射时间为60min,溅射温度为120℃,氩气流量为120sccm;
E.对表面镀覆有Ag/DLC复合薄膜的镁合金材料进行热处理,以消除薄膜应力。
实施例7
一种金属/DLC复合薄膜的制备方法,包括以下步骤:
A.选用镁合金为基体材料,将其切割为20×20×5mm;
B.依次用无水乙醇、去离子水超声清洗镁合金基体5min,然后烘干待用;
C.选用Cu/石墨复合靶材(其中金属铜的含量为9.8at.%),对复合靶材进行反溅射以清除表面的氧化物杂质;
D.将镁合金放入磁控溅射镀膜机中,抽真空使本底真空度低于5Pa,通入氩气为工作气体,开启溅射电源,对镁合金基体进行磁控溅射,其中靶基距为50mm,溅射功率为380W,溅射时间为60min,溅射温度为120℃,氩气流量为120sccm;
E.对表面镀覆有Cu/DLC复合薄膜的镁合金材料进行热处理,以消除薄膜应力。
实施例8
一种金属/DLC复合薄膜的制备方法,包括以下步骤:
A.选用镁合金为基体材料,将其切割为20×20×5mm;
B.依次用无水乙醇、去离子水超声清洗镁合金基体5min,然后烘干待用;
C.选用Cu/Ag/石墨复合靶材(其中金属银的含量为3.8at.%,金属铜的含量为6.0at.%),对复合靶材进行反溅射以清除表面的氧化物杂质;
D.将镁合金放入磁控溅射镀膜机中,抽真空使本底真空度低于5Pa,通入氩气为工作气体,开启溅射电源,对镁合金基体进行磁控溅射,其中靶基距为50mm,溅射功率为380W,溅射时间为60min,溅射温度为120℃,氩气流量为120sccm;
E.对表面镀覆有Cu/Ag/DLC复合薄膜的镁合金材料进行热处理,以消除薄膜应力。
对实施例1-8的抗菌性能进行测试,测试方法为:选择菌液浓度为8×105cfu/ml的金黄色葡萄球菌作为试验用菌液,分别取0.2ml试验用菌液滴加在样品表面,在37℃、相对湿度RH>90%的条件下,培养48h,然后取出样品进行活菌计数,并通过计数得到抗菌率。每个样品做5个平行试验,另外选择仅覆有DLC薄膜的镁合金为对照组。其中,抗菌率计算公式为:
R(%)=(A-B)/A×100
式中:R表示抗菌率;
A表示对照组平均回收菌数;
B表示实施例样品平均回收菌数。
实施例1-8及对照组的抗菌率如表1所示。
表1 抗菌率实验数据
实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 | 实施例7 | 实施例8 | |
抗菌率/% | 82.53 | 79.67 | 70.59 | 76.21 | 98.26 | 89.54 | 85.44 | 87.34 |
从表1可以看出,在DLC涂层中添加了Ag和/或Cu后都能够使其获得优异的抗菌性能,并且,在添加量相同的情况下,元素Ag的抗菌效果比元素Cu的抗菌效果更佳,并且,一定范围内,随着抗菌元素的添加量的增加,复合涂层的抗菌性能也得到提高。
令人惊讶的是,实施例5(6.0at.%Ag/3.8at.%Cu)的抗菌率提高到了预料之外的98.26%,其原因在于特定含量的铜/银添加量发生了协同效应,为了论证上述观点,发明人针对性地进行了实施例6(9.8at.%Ag)、实施例7(9.8at.%Cu)以及实施例8(3.8at.%Ag/6.0at.%Cu),实验结果证明,实施例6-8的抗菌性能都远远不如实施例5。这一发现,使得在某些对抗菌性能要求极高的情况下,实施例5中优异的抗菌效果可以得到应用。
Claims (6)
1.一种镁合金表面的金属/DLC复合薄膜,所述金属/DLC复合薄膜由磁控溅射法制备而得,其特征在于:所述磁控溅射法选用金属/石墨复合靶材,其中金属含量为3.8 at.%-9.8at.%,余量为石墨;所述金属为Ag和Cu。
2.一种如权利要求1所述的镁合金表面的金属/DLC复合薄膜,其特征在于:所述复合靶材中金属Ag的含量为6 at.%,金属铜的含量为3.8 at.%。
3.一种权利要求1或2所述的镁合金表面的金属/DLC复合薄膜的制备方法,其特征在于:包括如下步骤:
A.选用镁合金为基体材料,将其切割为20×20×5mm;
B.依次用无水乙醇、去离子水超声清洗镁合金基体5-10min,然后烘干待用;
C.选用金属/石墨复合靶材,对复合靶材进行反溅射以清除表面的氧化物杂质;
D.将镁合金放入磁控溅射镀膜机中,抽真空使本底真空度低于5Pa,通入氩气为工作气体,开启溅射电源,对镁合金基体进行磁控溅射,其中靶基距为40-50mm,溅射功率为380-450W,溅射时间为60-90min,溅射温度为100-120℃,氩气流量为120-150sccm;
E.对表面镀覆有Cu/Ag/DLC复合薄膜的镁合金材料进行热处理,以消除薄膜应力。
4.一种如权利要求3所述的镁合金表面的金属/DLC复合薄膜的制备方法,其特征在于:所述复合靶材中金属含量为3.8 at.%-9.8 at.%,余量为石墨;所述金属为Ag和Cu。
5.一种如权利要求4所述的镁合金表面的金属/DLC复合薄膜的制备方法,其特征在于:所述复合靶材中金属Ag的含量为6 at.%,金属铜的含量为3.8 at.%。
6.一种如权利要求4-5中任一项所述的镁合金表面的金属/DLC复合薄膜的制备方法,其特征在于:所述镁合金为医用镁合金。
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