CN113106520B - 一种碳化钽增强聚醚醚酮复合涂层及其制备方法与应用 - Google Patents

一种碳化钽增强聚醚醚酮复合涂层及其制备方法与应用 Download PDF

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CN113106520B
CN113106520B CN202110324850.7A CN202110324850A CN113106520B CN 113106520 B CN113106520 B CN 113106520B CN 202110324850 A CN202110324850 A CN 202110324850A CN 113106520 B CN113106520 B CN 113106520B
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林志丹
曹琳
张鹏
黄素媛
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Abstract

本发明属于生物材料技术领域，具体公开了一种碳化钽增强聚醚醚酮复合涂层及其制备方法与应用。所述方法包括以下步骤：(1)将壳聚糖溶液、乙醇混合均匀后，依次加入PEEK粉和纳米TaC得到混合溶液，经超声分散得到纳米悬浮液；(2)将阴极和阳极电极材料放入步骤(1)所得纳米悬浮溶液中；并通入直流电，沉积得到纳米TaC增强聚醚醚酮复合涂层。本发明通过阴极电沉积法在钛及其合金、不锈钢等基体上制备PEEK涂层，并在PEEK材料中引入纳米TaC粒子。可以增强PEEK的成骨性能。阴极电沉积制备的涂料生产时间短，设备简单，价格低廉，应用前景广阔。

Description

一种碳化钽增强聚醚醚酮复合涂层及其制备方法与应用
技术领域
本发明属于生物材料技术领域，特别涉及一种碳化钽增强聚醚醚酮复合涂层及其制备方法与应用。
背景技术
人工关节置换材料中钛及其合金具有优异的性能，例如低密度，高比强度，良好的耐电化学腐蚀性能，相对较低的弹性模量和良好的生物相容性。在生物医学工程中应用较广。钛及其合金具有密度低、特异强度高、电化学耐腐蚀性好、弹性度低、生物相容性好等优点。它们经常被用作航空航天、汽车、石化和海洋工业以及化学和生物医学工程中的结构部件。所有钛合金的主要缺点是耐磨损性差，摩擦系数(COF)高以及硬度相对较低。应用于关节磨损结构中时，容易造成离子溶出及应力屏蔽，导致骨溶解植入失败。理想的人工关节，应该满足一定力学支撑的基础上，耐磨和耐体液腐蚀。
聚醚醚酮具有优异的韧性和刚性，良好的热化学稳定性良好的摩擦学性能。但是纯PEEK在人体中作为称重结构使用时，机械强度不足，因此为提高其机械强度和成骨性能。
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碳化钽增强聚醚醚酮复合涂层的制备方法。
本发明另一目的在于提供上述方法制备得到的碳化钽增强聚醚醚酮复合涂层。
本发明再一目的在于提供所述碳化钽增强聚醚醚酮复合涂层在制备骨材料中的应用。
本发明的目的通过下述方案实现：
一种碳化钽增强聚醚醚酮复合涂层的制备方法，包括以下步骤：
(1)将壳聚糖溶液、乙醇混合均匀后，依次加入PEEK和纳米TaC得到混合溶液，经超声分散得到纳米悬浮液；
(2)将阴极和阳极电极材料放入步骤(1)所得纳米悬浮溶液中；并通入直流电，沉积得到碳化钽增强聚醚醚酮复合涂层。
步骤(1)乙醇：壳聚糖溶液的体积比为1～2：2～1；
步骤(1)壳聚糖溶液的浓度为0.5～0.1wt％。
步骤(1)混合溶液中所述PEEK含量为1-4wt％；所述TaC添加量为0.01-3wt％，优选为0.1wt％。
步骤(1)混合溶液中所述PEEK粒径为20-30μm，纳米TaC粒径为50-100nm。
步骤(2)所述阴极材料为钛合金、纯钛或不锈钢；优选地，在使用阴极材料前，先对其进行清洗，具体为对表面进行喷砂处理，形成一粗糙面，用无水酒精、丙酮清洗。所述阳极材料为常用惰性电极，优选为石墨或铂片。
步骤(2)中所述直流电的电压为10～30V，优选为25V；所述电流的密度为0.01-0.05A/cm2。所述电极之间的距离为1-3cm，优选为1cm；所述沉积时间为1-5min。
一种碳化钽增强聚醚醚酮复合涂层通过上述方法制备得到。
所述碳化钽增强聚醚醚酮复合涂层在制备成骨材料中的应用。
本发明相对于现有技术，具有如下的优点及有益效果：
本发明通过阴极电沉积法在钛及其合金、不锈钢等基体上制备PEEK涂层，并在PEEK材料中引入碳化钽纳米粒子。TaC可以吸附在PEEK颗粒上，沉积涂层更加密实，可以改善钛合金的耐磨性能，改善PEEK材料的硬度，增强PEEK的成骨性能。阴极电沉积制备的涂料生产时间短，设备简单，价格低廉，应用前景广阔。
附图说明
图1为实施例5所得涂层的TEM图。
图2中(a)和(b)为实施例5所得涂层的SEM图，(c)为元素分布图。
具体实施方式
下面结合实施例和附图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1-11中TaC增强聚醚醚酮复合涂层采用以下方法制得：
(1)壳聚糖溶液：将0.5g壳聚糖、5mL冰乙酸和500mL去离子水混合；
(2)将上述50mL壳聚糖溶液与50mL乙醇混合均匀，然后加入1～5gPEEK粉(20-30μm)和0.01～0.2g TaC(50-100nm)，得到混合溶液；
(3)将步骤(2)所得混合溶液经超声分散20min、搅拌溶解7h，得到纳米悬浮溶液。
(4)将阴极(纯钛)和阳极(Pt)电极材料放入步骤(3)所得纳米悬浮溶液中，电极间距1-2cm；并通入直流电，施加电压15-20V，电流密度0.01-0.5mA/cm2，沉积1-5min得到碳化钽增强聚醚醚酮复合涂层。
表1实施例1～11的条件参数及所得涂层的性能
Figure BDA0002994170450000031
Figure BDA0002994170450000041
TaC是一种大小不一的球形纳米颗粒，具有较强硬度和极高的稳定性。本发明加入适量TaC后，其在沉积液中与PEEK吸附在一起，共沉积。如表1所示能够提升材料的摩擦性能，比如摩擦系数明显降低(在摩擦过程中滚动滑动的作用，减少材料的接触的力)，磨损率明显减少，磨损深度降低。因为是纳米粒子，所以在添加到PEEK基体后，经过烧结形成复合材料的时候能够提高PEEK的结晶性能，使得材料整体性能改变，比如说硬度提高。至于耐刮擦，因为在PEEK材料中是均匀分布的(电沉积可以做到均匀分布)，所以也同时提高了材料的硬度，在刮擦过程中可以分散应力，起到保护作用。
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 (7)

1.一种碳化钽增强聚醚醚酮复合涂层的制备方法，其特征在于包括以下步骤：
(1)将壳聚糖溶液、乙醇混合均匀后，依次加入PEEK和纳米TaC得到混合溶液，经超声分散得到纳米悬浮液；
(2)将阴极和阳极电极材料放入步骤(1)所得纳米悬浮溶液中；并通入直流电，沉积得到碳化钽增强聚醚醚酮复合涂层；
步骤(1)混合溶液中所述PEEK含量为3g；所述TaC添加量为0.05g；
步骤(1)壳聚糖溶液的制备方法为将0.5g壳聚糖、5mL冰乙酸和500mL去离子水混合；
控制电流为0.025A/cm2，沉积时间为2min。
2.根据权利要求1所述的制备方法，其特征在于：步骤(1)乙醇：壳聚糖溶液的体积比为1～2：2～1。
3.根据权利要求1所述的制备方法，其特征在于：步骤(1)混合溶液中所述PEEK粒径为20-30μm，纳米TaC粒径为50-100nm。
4.根据权利要求1所述的制备方法，其特征在于：步骤(2)中直流电的电压为10～30V；步骤(2)中电极之间的距离为1-3cm。
5.根据权利要求1所述的制备方法，其特征在于：步骤(2)所述阴极材料为钛合金、纯钛或不锈钢；所述阳极材料为常用惰性电极。
6.一种碳化钽增强聚醚醚酮复合涂层，通过权利要求1～5任一项所述方法制备得到。
7.根据权利要求6所述的碳化钽增强聚醚醚酮复合涂层在制备成骨材料中的应用。
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Inventor after: Cao Lin

Inventor after: Zhang Peng

Inventor after: Lin Zhidan

Inventor after: Huang Suyuan

Inventor before: Lin Zhidan

Inventor before: Cao Lin

Inventor before: Zhang Peng

Inventor before: Huang Suyuan