CN107137766B - 抗菌型人工关节固定界面的制备方法 - Google Patents

抗菌型人工关节固定界面的制备方法 Download PDF

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CN107137766B
CN107137766B CN201710303525.6A CN201710303525A CN107137766B CN 107137766 B CN107137766 B CN 107137766B CN 201710303525 A CN201710303525 A CN 201710303525A CN 107137766 B CN107137766 B CN 107137766B
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titanium alloy
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CN107137766A (zh
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陈凯
张德坤
杨雪晖
魏生
许林敏
葛世荣
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China University of Mining and Technology CUMT
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Abstract

本发明公开了一种抗菌型人工关节固定界面的制备方法，工艺：1)将医用钛合金试样表面制备出微孔结构；2)将带有微孔结构的医用钛合金试样浸泡在重铬酸氧化溶液中氧化，结束后用氧离子束处理，在表面覆盖硅烷溶液；3)按质量百分比制备出羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液，加入到带有微孔结构的医用钛合金试样表面，并使羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液达到10μm‑100μm；4)将医用钛合金试样放入透明玻璃箱中密封，并将其置于阴暗处自然干燥一周；5)最后将带有羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石复合水凝胶的医用钛合金试样置于50℃下的烘干箱内干燥24h，即可制得抗菌型人工关节固定界面。

Description

抗菌型人工关节固定界面的制备方法
技术领域
本发明属于人工关节技术领域，具体涉及一种人工关节生物固定界面制备工艺，特别是一种抗菌型人工关节生物固定界面的制备工艺。
背景技术
人工关节置换术自上世纪60年代广泛应用于临床以来，已成为治疗人类关节毁损最成功、最有效的外科和康复手段。全球约有4亿人患有严重的骨关节疾病，其中我国就超过1亿患者，每年需要人工关节置换约200万例。但是，目前的人工关节假体仍然存在一些问题，难以满足日益增长的高可靠性、长寿命人工关节置换需求。其主要原因是植入假体的抗磨损、强固定、抗感染等关键技术尚未得到很好的解决。
虽然人工关节置换已成为临床治疗关节疾病或创伤的有效途径，但是由于人工植入材料不具备自然界生命力的代谢作用，假体界面行为与生命介质的相容性差，随着全球人口老龄化和关节置换病人的年轻化趋势，目前人工关节还远达不到20年乃至30年不翻修的期望目标。统计表明关节手术失败的前四大主要因素是：磨损、松动、失稳、感染。其中，磨损和松动是引起关节晚期失效的主要原因，而感染是造成关节早期失效的主要原因。如何解决以上科学技术难题，是当今国际人工关节置换领域的研究热点和趋势。
因此，设计抗菌型人工关节生物固定界面，制造防松动、抗感染的人工关节，是解决人工关节无菌性松动和感染问题的最佳选择，这也将有助于延长人工关节假体的使用寿命，降低假体置换者的痛苦或危险，这对于提高假体置换者的生命质量、推动我国的植入体制造产业的发展具有重要意义。
综上所述，制备具有抗菌特性的人工关节是未来的发展趋势。
发明内容
发明目的：为了克服现有技术中存在的不足，本发明提供一种抗菌型人工关节固定界面的制备工艺，通过该方法获得一种具有抗菌特性的仿生人工关节固定界面，解决植入假体的固定、感染等问题。
技术方案：为实现上述目的，本发明采用的技术方案为：
一种抗菌型人工关节固定界面的制备方法，包括以下步骤：
1)医用钛合金试样进行表面激光处理，将其表面制备出微孔结构；
2)将带有微孔结构的医用钛合金试样清洁后，浸泡在重铬酸氧化溶液中进行氧化，结束后用氧离子束处理，并在表面覆盖硅烷溶液；
3)制备羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液，加入到步骤2)处理后的医用钛合金试样表面；
4)将医用钛合金试样放入透明玻璃箱中密封，并将其置于阴暗处自然干燥一周；
5)最后将带有羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石复合水凝胶的医用钛合金试样置于50℃下的烘干箱内干燥24h，即可制得抗菌型人工关节固定界面。
进一步的，步骤2)的具体方法为：将清洁后的带有微孔结构的医用钛合金试样浸泡在重铬酸氧化溶液中，并置于75℃水浴锅中10min，取出用去离子水清洗；然后将带有微孔结构的医用钛合金试样表面用氧离子束在200真空度、30W条件下处理5min；在带有微孔结构的医用钛合金试样表面覆盖硅烷溶液，在室温下浸泡2h；然后用乙醇清洗，干燥后储存在低湿度环境下。
进一步的，所述硅烷溶液由100ml去离子水、10ml pH3.5的乙醇和2wt％γ-甲基丙烯酰氧丙基三甲氧基硅烷混合制备而成。
进一步的，步骤3)的具体方法为：按质量百分比称取羧甲基壳聚糖3％、明胶1％、纳米银0.1％、纳米羟基磷灰石1％、去离子水94.9％，将其置于55℃水浴锅中，制备出羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液，将制备好的羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液加入到步骤2)处理后的带有微孔结构的医用钛合金试样表面。
进一步的，羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液达到10μm-100μm的厚度。
根据上述的方法制备的抗菌型人工关节固定界面，抗菌型人工关节固定界面的接触角为26°。
有益效果：本发明提供的抗菌型人工关节固定界面的制备方法，采用上述技术方案，抗菌水凝胶在医用钛合金试样表面上，两者之间结合良好，并表现出良好的抗菌效果，达到了本发明的目的，实现了抗菌型人工关节固定界面的制造，对于抗感染人工关节的制造具有重要意义，这对于提高假体置换者的生命质量、推动我国的植入体制造产业的发展具有重要意义。
附图说明
图1为本发明的制备原理图。
图2为本发明的抗菌型人工关节固定界面的润湿性能图，其中，图2(a)所示为医用钛合金试样，图2(b)所示为氧化处理后的钛合金试样，图2(c)所示覆盖抗菌水凝胶后的钛合金试样。
具体实施方式
下面结合附图对本发明作更进一步的说明。
本发明为一种抗菌型人工关节固定界面的制备方法，工艺如下：1)利用精密激光打孔机将医用钛合金试样表面制备出微孔结构；2)将带有微孔结构的医用钛合金试样浸泡在重铬酸氧化溶液中进行氧化，结束后用氧离子束处理，然后在带有微孔结构的医用钛合金试样表面覆盖硅烷溶液；3)按质量百分比制备出羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液，将制备好的羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液加入到步骤2处理后的带有微孔结构的医用钛合金试样表面，并使羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液达到一定的厚度；4)将医用钛合金试样放入透明玻璃箱中密封，并将其置于阴暗处自然干燥一周；5)最后将带有羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石复合水凝胶的医用钛合金试样置于50℃下的烘干箱内干燥24h，即可制得抗菌型人工关节固定界面。
实施例
如图1所示，一种抗菌型人工关节固定界面制备工艺的具体步骤如下：
1)表面激光处理：利用精密激光打孔机将医用钛合金试样表面制备出微孔结构，用丙酮、乙醇和去离子水按顺序彻底清洗带有微孔结构的医用钛合金试样，如图2(a)所示为医用钛合金试样；
2)表面氧化处理及硅烷处理：将清洁后的带有微孔结构的医用钛合金试样浸泡在重铬酸氧化溶液(重铬酸钾与浓硫酸按质量百分比1:4)中，并置于75℃水浴锅中10min，取出用大量去离子水进行清洗；然后将带有微孔结构的医用钛合金试样表面用氧离子束处理5分钟(200真空度，30W)；立即在带有微孔结构的医用钛合金试样表面覆盖硅烷溶液(100ml的去离子水，10ml pH3.5的乙醇和2wt％γ-甲基丙烯酰氧丙基三甲氧基硅烷)，在室温下浸泡2h；然后用乙醇将带有微孔结构的清洗，完全干燥后储存在低湿度环境下，如图2(b)所示为为氧化处理后的钛合金试样。
3)覆盖抗菌水凝胶：按质量百分比称取的羧甲基壳聚糖3％、明胶1％、纳米银0.1％、纳米羟基磷灰石1％、去离子水94.9％，将其置于55℃水浴锅中，制备出羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液，将制备好的羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液加入到步骤2)处理后的带有微孔结构的医用钛合金试样表面，并使羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液达到10μm-100μm之间，主要是考虑抗菌效果和降解速度，因此选择一个范围，实现降解与抗菌的可控性，如图2(c)所示覆盖抗菌水凝胶后的钛合金试样。
4)干燥处理：将按以上方法处理过后的医用钛合金试样放入透明玻璃箱中密封，并将其置于阴暗处自然干燥一周。
5)最后将带有羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石复合水凝胶的医用钛合金试样置于50℃下的烘干箱内干燥24h，即可制得抗菌型人工关节固定界面。
原始医用钛合金试样的接触角为70°，经过氧化处理后医用钛合金试样的接触角变为42°，最后覆盖抗菌水凝胶后的接触角为26°，较小的接触角有利于细胞生长和人工关节的固定。抗菌型人工关节固定界面具有良好的亲水性能，接触角仅为26°，抗菌水凝胶与医用钛合金之间的结合强度大于1MPa，两者不会发生脱落，抗菌型人工关节固定界面对大肠杆菌和金黄色葡萄球菌表现出了良好的抗菌效果，并且抗菌型人工关节固定界面具有良好的降解性能，可根据界面的厚度实现降解时间的调控。
以上所述仅是本发明的优选实施方式，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。

Claims (3)

1.一种抗菌型人工关节固定界面的制备方法，其特征在于：包括以下步骤：
1）医用钛合金试样进行表面激光处理，将其表面制备出微孔结构；
2）将带有微孔结构的医用钛合金试样清洁后，浸泡在重铬酸氧化溶液中进行氧化，结束后用氧离子束处理，并在表面覆盖硅烷溶液；
3）制备羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液，加入到步骤2）处理后的医用钛合金试样表面；
4）将医用钛合金试样放入透明玻璃箱中密封，并将其置于阴暗处自然干燥一周；
5）最后将带有羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石复合水凝胶的医用钛合金试样置于50℃下的烘干箱内干燥24h，即可制得抗菌型人工关节固定界面；
步骤2）的具体方法为：将清洁后的带有微孔结构的医用钛合金试样浸泡在重铬酸氧化溶液中，并置于75℃水浴锅中10min，取出用去离子水清洗；然后将带有微孔结构的医用钛合金试样表面用氧离子束在200真空度、30W条件下处理5min；在带有微孔结构的医用钛合金试样表面覆盖硅烷溶液，在室温下浸泡2h；然后用乙醇清洗，干燥后储存在低湿度环境下；
所述硅烷溶液由100ml去离子水、10ml pH3.5的乙醇和2wt% γ-甲基丙烯酰氧丙基三甲氧基硅烷混合制备而成；
步骤3）的具体方法为：按质量百分比称取羧甲基壳聚糖3%、明胶1%、纳米银0.1%、纳米羟基磷灰石1%、去离子水94.9%，将其置于55℃水浴锅中，制备出羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液，将制备好的羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液加入到步骤2）处理后的带有微孔结构的医用钛合金试样表面。
2.根据权利要求1所述的抗菌型人工关节固定界面的制备方法，其特征在于：羧甲基壳聚糖/明胶/纳米银/纳米羟基磷灰石溶液达到10μm-100μm的厚度。
3.根据权利要求1或2所述的方法制备的抗菌型人工关节固定界面，其特征在于：抗菌型人工关节固定界面的接触角为26°。
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