CN115341255A - 一种离子注入PEEK-Cu复合涂层及其制备方法与应用 - Google Patents
一种离子注入PEEK-Cu复合涂层及其制备方法与应用 Download PDFInfo
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Abstract
本发明属于生物植入材料技术领域，特别涉及一种离子注入PEEK‑Cu复合涂层及其制备方法与应用。所述方法将TaB2和PEEK的混合颗粒在壳聚糖悬浮液中分散均匀得到电泳沉积液；在阴极沉积后所得样品进行热处理，再进行铜离子注入，得到最终复合涂层。本发明通过等离子体浸没离子注入将不同剂量Cu(1×1017ions/cm2、3×1017ions/cm2、6×1017ions/cm2)引入TaB2/PEEK复合材料表面，获得具有持续性抗菌效果的成骨的材料。
Description
技术领域
本发明属于生物植入材料技术领域，特别涉及一种离子注入PEEK-Cu复合涂层及其制备方法与应用
背景技术
人工关节置换术后最为严重的并发症就是人工关节假体周围感染。植入的假体材料与骨骼之间存在间隙，如果细菌粘附速度比宿主组织再生速度更快，将导致骨关节假体相关性感染的发生。防止细菌粘附对于预防植入物相关性感染至关重要，现有技术证明TaB2/PEEK(硼化钽/聚醚醚酮)材料具有良好的摩擦学和生物相容性，具有促进巨噬细胞向M2分化的倾向，但TaB2和PEEK材料本身不具备抗菌性能，所以开发具有抗菌性能的TaB2/PEEK复合材料，以促进细胞粘附、增殖同时抑制细菌粘附和生长具有重要意义。
铜是人体必需的微量元素，铜抗菌元素具有良好的抗菌作用，是体内外有效的抗菌剂，但摄入过量的铜可能会导致细胞氧化损伤和细胞死亡。使用传统的沉积方法(如磁控溅射、线弧沉积)在聚合物基质上沉积一层铜薄膜是一项挑战，这些方法涉及的工作温度非常高。此外PEEK与铜的并不能很好的结合，无法对铜起到缓释的效果。
发明内容
为了克服上述现有技术的缺点与不足，本发明的首要目的在于提供一种离子注入PEEK-Cu复合涂层的制备方法。
本发明另一目的在于提供一种离子注入PEEK-Cu复合涂层。
本发明再一目的在于提供所述离子注入PEEK-Cu复合涂层在制备仿生材料中的应用。
本发明的目的通过下述方案实现：
一种离子注入PEEK-Cu复合涂层的制备方法，包括以下步骤：
(1)将TaB2和PEEK的混合颗粒在壳聚糖悬浮液中分散均匀得到电泳沉积液；
(2)在电泳沉积液中进行电泳沉积，在阴极上沉积TaB2/PEEK复合涂层；
(3)将沉积TaB2/PEEK的样品进行热处理，随炉冷却；
(4)将Cu靶放入阴极电弧源，步骤(3)所得样品放置于样品台抽真空，然后将氩气以引入阴极电弧源，通过施加脉冲负高压注入铜离子，得到离子注入PEEK-Cu复合涂层。
步骤(1)所述壳聚糖悬浮液的浓度为0.5～3g/L。
步骤(1)电泳沉积液中TaB2的浓度为1～5wt％，优选为3wt％；PEEK的浓度为1～5wt％，优选为2.5wt％。
步骤(2)所述电泳沉积的外加电压为10-20V，外加电压时间为10-240s，优选为60～120s。
步骤(3)所述热处理的温度为350～450℃，热处理的时间为40～90min。
步骤(4)所述铜离子的注入剂量为1.0～6.0×1017ions·cm-2。
一种离子注入PEEK-Cu复合涂层，由上述方法制备得到的。
所述离子注入PEEK-Cu复合涂层在制备仿生材料中的应用。
本发明相对于现有技术，具有如下的优点及有益效果：
本发明通过PIII技术(等离子体浸没离子注入)将不同剂量Cu(1×1017ions/cm2、3×1017ions/cm2、6×1017ions/cm2)引入TaB2/PEEK复合材料表面，获得具有持续性抗菌效果的成骨的材料。
附图说明
图1中(a)-(d)为PTB3/390与抗菌复合材料的SEM图；(a`)-(d`)为(a)-(d)的局部放大图；(a``)-(d``)为Cu的元素分布图。
具体实施方式
下面结合实施例对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例中所用试剂如无特殊说明均可从市场常规购得。
实施例中抗菌效果表征操作如下：
本试验使用金黄色葡萄球菌(Staphylococcus aureus,S.aureus)和大肠杆菌(Escherichia coli,E.coli),根据中国国家标准JISZ 2801-2000、ISO 22196、GB/T31402-2015平板计数法评估PTB3/390和不同注入剂量的铜抗菌复合材料的抗菌能力。
将不同材料(15mm×10mm×2mm)121℃高压灭菌30min，细菌接种前将样品浸泡在PBS中10min后吸弃。将1mL浓度为1×105cfu/mL菌液(共培养6h)、1×106cfu/mL(共培养24h)菌液加入样品孔中，在摇床中分别在共培养。每组设置3个平行试验样品。
按照时间节点将菌液吸出，使用PBS稀释至浓度为1×104cfu/mL，取30μL均匀涂布在琼脂表面，随后放入37℃恒温培养箱中培养18h，按照时间节点取出拍照。每个样品设置3组平行试验组。计算抗菌率。
实施例1
一种离子注入PEEK-Cu复合涂层的制备方法，包括以下步骤：
(1)对纯钛片(TA2)进行喷砂处理，随后在乙醇中超声清洗3次备用。
(2)将壳聚糖粉末溶解在1vol％冰乙酸水溶液中，在室温下以500rpm磁力搅拌24h，获得1g/L壳聚糖悬浮液。将3wt％TaB2和2.5wt％PEEK颗粒电泳沉积液超声处理30min并磁力搅拌24h，直至TaB2和PEEK颗粒充分分散在沉积液中。
(3)阴极(TA2)和阳极对电极(铂，3×3cm)之间的距离恒定在10mm。采用反复实验的方式对EPD过程中的外加电压和时间进行调整，使用15V，100s的沉积时间进行材料沉积。为了避免颗粒沉降，EPD过程中持续对EPD液进行磁力搅拌。
(4)将TaB2/PEEK样品在管式炉中，空气气氛下，以4.5℃/min的速率分别升温至目标温度390℃，并保温60min，随炉冷却。
(5)在进行等离子体注入前将样品在乙醇中超声清洗。纯Cu靶放入阴极电弧源，将样品放置于样品台抽真空至5×10-4Pa，将氩气(Ar)以6sccm(标准立方厘米每分钟)的流速引入阴极电弧源。通过施加脉冲负高压注入铜离子。注入计量分别为1.0×1017、3.0×1017、6.0×1017ions·cm-2，得到Cu/TaB2/PEEK材料，分别记为PTB3/390/1Cu、PTB3/390/3Cu、PTB3/390/6Cu。
对比例1
本对比例与实施例1的区别在于不包括步骤(5)。所得样品记为PTB3/390对比例2
本对比例与实施例1的区别在于步骤(2)中不加入TaB2颗粒。所得样品记为PEEK/390/1Cu
由图1可以看到，离子注Cu后表面的Cu元素以Cu2O和CuO的形式存在。且Cu元素主要存在于涂层内部，因此会对铜离子的缓释有积极作用。
表1不同样品与细菌工培养6h和24h后的抗菌率
由表1可知，本发明所得铜复合抗菌材料具有良好的抗菌效果，铜复合抗菌材料的抗菌作用可能与材料中释放的Cu+和Cu2+离子有关。当铜复合抗菌材料与金黄色葡萄球菌和大肠杆菌共培养时，样品中释放的铜离子迅速将细胞膜破坏，与蛋白质中的巯基结合，使细菌呼吸所需的ATP酶无法合成，导致细菌死亡。而当材料中不加入TaB2时，PEEK/390/1Cu的抗菌效果减弱，且无法对Cu离子持续性释放，而不注入Cu时，PTB3/390的抗菌效果不到40％。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (10)
1.一种离子注入PEEK-Cu复合涂层的制备方法，其特征在于包括以下步骤：
(1)将TaB2和PEEK的混合颗粒在壳聚糖悬浮液中分散均匀得到电泳沉积液；
(2)在电泳沉积液中进行电泳沉积，在阴极上沉积TaB2/PEEK复合涂层；
(3)将沉积TaB2/PEEK的样品进行热处理，随炉冷却；
(4)将Cu靶放入阴极电弧源，步骤(3)所得样品放置于样品台抽真空，然后将氩气以引入阴极电弧源，通过施加脉冲负高压注入铜离子，得到离子注入PEEK-Cu复合涂层。
2.根据权利要求1所述的方法，其特征在于：步骤(1)所述壳聚糖悬浮液的浓度为0.5～3g/L。
3.根据权利要求1所述的方法，其特征在于：步骤(1)电泳沉积液中TaB2的浓度为1～5wt％。
4.根据权利要求1所述的方法，其特征在于：步骤(1)电泳沉积液中PEEK的浓度为1～5wt％。
5.根据权利要求1所述的方法，其特征在于：步骤(1)电泳沉积液中TaB2的浓度为3wt％，PEEK的浓度为2.5wt％。
6.根据权利要求1所述的方法，其特征在于：步骤(2)所述电泳沉积的外加电压为10-20V，外加电压时间为10-240s。
7.根据权利要求1所述的方法，其特征在于：步骤(3)所述热处理的温度为350～450℃，热处理的时间为40～90min。
8.根据权利要求1所述的方法，其特征在于：步骤(4)所述铜离子的注入剂量为1.0～6.0×1017ions·cm-2。
9.一种离子注入PEEK-Cu复合涂层，由权利要求1～8任一项所述方法制备得到。
10.权利要求9所述离子注入PEEK-Cu复合涂层在制备仿生材料中的应用。
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