CN116570766A - Ag-TiO2 -OTS疏水涂层的制备方法及其作为抗菌种植体的应用 - Google Patents
Ag-TiO2 -OTS疏水涂层的制备方法及其作为抗菌种植体的应用 Download PDFInfo
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Abstract
本发明提供一种具备杀菌和疏水能力的种植体材料。其中以Ti为基体，利用化学镀的方法将二氧化钛(TiO2)和十八烷基三氯硅烷(OTS)掺入银(Ag)纳米材料涂层内，制备双纳米颗粒协同修饰Ti的复合涂层，利用Ag的广谱杀菌性能，TiO2的光催化降解效果和OTS的超疏水性从物理方法直接抑制细菌附着，形成具备杀菌和抗吸附能力的复合涂层，更加高效持久防止植入体感染。本发明提供所述Ag‑TiO2‑OTS复合涂层的制备方法及其作为抗菌植入体的应用。本发明所述的复合涂层对大肠杆菌和金黄色葡萄球菌均具备抗吸附能力。
Description
技术领域
本发明涉及生物种植体材料领域，Ag-TiO2-OTS涂层具备疏水效果，能够减少细菌在种植体表面的吸附繁殖，从而降低种植体的术后感染率。
背景技术
在现代医疗背景下，种植体在骨科、牙科、整形外科等领域的应用越来越广泛，同时种植体材料所引发的相关感染问题也日趋严重。研究指出多达80％的生物医疗材料引发的感染是由于生物膜附着在材料表面所致，种植体植入到受创伤的皮肤或组织，创伤处很容易受到细菌的入侵形成生物膜。一旦生物膜在材料表面上生成，细菌更易于侵入，使防御机制降低进而促进细菌的粘附、繁殖形成感染，最终导致手术失败。
钛(Ti)及其合金因为良好的生物相容性、优异的机械强度和良好的耐腐蚀性而被广泛应用为植入体材料，但并不具备抗菌效果，因此要对其表面进行修饰。
银(Ag)和二氧化钛(TiO2)这种金属与光催化材料的联合应用也十分广泛，Ag作为广谱杀菌剂的应用已有长久的历史，TiO2在可见光下由于电子-空穴对的分离和复合产生活性氧，起到杀菌作用。当两者联用时，银离子能够延长TiO2的电子-空穴对的分离复合过程，从而提高了抗菌效果。但细菌接触到种植体表面仍然会形成生物膜，从而阻隔杀菌剂和菌的接触，不能继续发挥杀菌作用。
十八烷基三氯硅烷(OTS)是一种长链硅烷，具有超疏水能力，在防冻、耐磨和抗菌等领域的应用已有一定成就。当它在种植体表面存在时，使得种植体具备疏水效果，细菌不易在其表面吸附定植，生物膜的生成也会相应减少。
本发明首先在Ti表面沉积Ag-TiO2涂层，使得种植体具备杀菌效果，再将OTS接枝到其表面，使得种植体同时具备物理性的抗菌吸附效果，降低种植体手术的感染。
发明内容
本发明目的在于制备一种具备杀菌能力，同时具备疏水能力的种植体材料。
为实现上述目的，Ag-TiO2-OTS疏水复合涂层的制备采用以下步骤。
1)Ti基体的打磨清洗。
2)Ag涂层的制备，将Ti悬挂银镜反应液中避光反应24h。
3)Ag-TiO2涂层的制备，将TiO2悬液加入避光反应了4h的Ag涂层制备反应液中，并以300rpm的速度搅拌继续反应。
4)Ag-TiO2-OTS复合涂层的制备，将正己烷加入制备的OTS反应液中，覆盖Ag-TiO2涂层的Ti基体过夜浸泡其中。
基于以上技术方案，本发明的Ag-TiO2-OTS复合涂层具备超疏水能力和抗菌能力，其制备具有工艺简单环保，条件温和，制备周期短等特点。
Ag涂层、Ag-TiO2涂层和Ag-TiO2-OTS复合涂层用于对大肠杆菌和金黄色葡萄球菌的抗吸附能力评估。
附图说明
图1为本发明实施例1中Ag-TiO2-OTS复合涂层的扫描电子显微镜(SEM)图。
图2为本发明实施例1中Ag-TiO2-OTS复合涂层的能量色散X射线光谱仪(EDX)图。
图3为本发明实施例1中Ag-TiO2-OTS复合涂层的X射线光电子能谱仪(XPS)图。
图4为本发明实施例1中Ti、Ag涂层、Ag-TiO2涂层和Ag-TiO2-OTS复合涂层的X射线衍射仪(XRD)图。
图5为本发明实施例1中Ag-TiO2-OTS复合涂层的原子力扫描探针显微镜(AFM)图。
图6为本发明实施例2中大肠杆菌在各组样品表面吸附情况分析。
图7本发明实例2中金黄色葡萄球菌在各组样品表面细菌情况分析。
具体实施方式
实施例1
1)Ti基体的处理：打磨光滑后，分别用1M盐酸、0.125M氢氧化钠溶液、丙酮和乙醇超声清洗后晾干，在冰浴条件下，清洗晾干后的Ti先浸泡于浓硫酸中3min，再加入与浓硫酸等体积的过氧化氢隔绝空气并浸泡5min，取出后用去离子水彻底冲洗干净并晾干，之后在紫外灯下双面照射90min。
2)Ag涂层的制备：0.276g硝酸银，0.192g氢氧化钠和6mL氨水混合后加入40mL去离子水避光，另配一份0.3168g水合葡萄糖和0.032g酒石酸钾钠的混合物，加入40mL去离子，两份溶液混合后将Ti悬挂其中避光反应24h。
3)Ag-TiO2涂层的制备：将0.16gTiO2粉末加入2mL去离子水并搅拌，在Ag涂层制备避光反应至4h时，加入TiO2悬液并以300rpm的速度搅拌继续反应。
4)Ag-TiO2-OTS复合涂层的制备：取1mLOTS，加入20μL去离子水，盖盖震荡10s，开盖状态下超声10s，再盖盖震荡10s，之后取500μL静置2h，之后加入正己烷10mL，将覆盖Ag-TiO2涂层的Ti基体过夜浸泡其中。对所得产物Ag-TiO2-OTS复合涂层进行SEM，EDX,XPS,FTIR及AFM表征，结果如图1、2、3、4、5所示。
实施例2
取Ti、Ag涂层、Ag-TiO2涂层和不同浓度OTS制备的疏水涂层浸泡在浓度为106的菌液中，在37℃，80rmp的条件下分别震荡培养1h、24h、72h和168h后，稀释至102并在琼脂板上涂布过夜培养，计算各组样品表面的细菌繁殖浓度。图6为各组样品表面大肠杆菌的生长情况，图7为金黄色葡萄球菌表面的生长情况。
以上具体实例，对本发明的目的、技术方案和应用进行了进一步详细说明。以上所述仅为本发明的具体实施例，并不用于限制本发明，凡在本发明的精神和原则之内，所做的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (7)
1.制备一种以Ti为基底的抗菌种植体材料。以Ti为基底，在其表面沉积Ag涂层，再镶嵌TiO2纳米颗粒，之后在表面接枝OTS形成表面疏水的复合纳米涂层，得到具备抗菌能力的纳米复合涂层材料。
2.根据权利要求1所述的Ag-TiO2-OTS复合涂层，其中Ti为直径1cm，厚度0.1cm的纯Ti圆片。
3.根据权利要求1所述的Ag-TiO2-OTS复合涂层，其中银的来源为硝酸银。
4.根据权利要求1所述的Ag-TiO2-OTS复合涂层，其中TiO2的纳米粒的粒径为20-200nm。
5.根据权利要求1所述的Ag-TiO2-OTS复合涂层，其中OTS的平均直径为200-400nm。
6.一种制备权利要求1所述Ag-TiO2-OTS复合涂层制备的方法：
1)将Ti在银镜反应溶液里悬挂，避光静置24h，得到Ag涂层。
2)将TiO2悬液加入1)中的反应液，并搅拌避光反应，得到Ag-TiO2涂层。
3)将Ag-TiO2涂层覆盖的Ti浸泡在OTS反应液和正己烷混合溶液中，得到Ag-TiO2-OTS复合涂层。
7.根据权利要求1所述的Ag-TiO2-OTS复合涂层的应用，其特征在于表面具有超疏水性，能阻止细菌吸附。
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