CN113737055B - 一种钛合金表面共掺杂抗菌/骨诱导材料及其制备方法 - Google Patents

一种钛合金表面共掺杂抗菌/骨诱导材料及其制备方法 Download PDF

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CN113737055B
CN113737055B CN202111047089.3A CN202111047089A CN113737055B CN 113737055 B CN113737055 B CN 113737055B CN 202111047089 A CN202111047089 A CN 202111047089A CN 113737055 B CN113737055 B CN 113737055B
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titanium alloy
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antibacterial
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夏木建
周广宏
刘磊
李年莲
朱雨富
丁红燕
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Huaiyin Institute of Technology
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Abstract

本发明公开了一种钛合金表面共掺杂抗菌/骨诱导材料及其制备方法，所述制备方法包括钛合金分别置于丙酮、无水乙醇中超声清洗；在水中加入硝酸银和纳米羟基磷灰石并混合均匀，所得的混合溶液经压力雾化器喷洒于上述清洗后的钛合金的表面上；在氮气气氛下，使用飞秒激光在钛合金的表面上扫描加工，得到钛合金表面共掺杂抗菌/骨诱导材料。本发明在钛合金表面采用氮气/雾化辅助一步法激光原位成形具有Ag‑N‑HA共掺杂TiO2微孔结构，能增强其与钛合金基体的膜/基结合强度，有效延长钛合金植入体的服役寿命。

Description

一种钛合金表面共掺杂抗菌/骨诱导材料及其制备方法
技术领域
本发明涉及一种钛合金材料及其制备方法，尤其涉及一种钛合金表面共掺杂抗菌/骨诱导材料及其制备方法。
背景技术
老年人口和骨科疾病患者对可植入生物医用材料的需求量正日益增加。作为骨植入体的材料应与人体自然骨具有相似的力学性及良好的生物相容性。相比于其它金属而言，钛及钛合金具有优良的生物相容性、良好的强度及疲劳等力学性能，且弹性模量和硬度均接近于皮质骨组织的性能，促使钛成为制造骨科植入体的理想材料。钛合金作为生物惰性金属材料，作为异物植入人体后，其表面易吸附蛋白质、细菌等物质，随着细菌生长和繁殖以及生物膜形成容易引起感染，而钛合金无抑菌功能，使得患者口服或静脉注射抗生素以减少感染，增加患者的经济和病痛。另一方面，钛合金自身无生活活性，难以促进钛合金骨植入体周围的骨组织生长，延长了患者的治愈周期。
当前，主要通过钛合金表面改性的方法在其表面构建膜层以解决上述问题。如在钛合金表面通过酯化反应合成Ag掺杂的含茶酚壳聚糖膜层，以提高其抗菌效果；通过等离子喷涂法、电泳沉积法等表面改性工艺在钛合金表面沉积HA或Ag掺杂HA涂层。上述方法在一定程度上提高了钛合金骨植入体的抗菌或骨诱导生长能力。但钛合金植入体在人体服役过程中必然承载自然骨传递的压应力作用，对钛合金表面改性涂层的膜/基结合强度提出了较高的要求，而抗菌或HA涂层与钛合金间物性差异大，易导致膜/基界面应力大，最终表现为涂层的过早失效。
发明内容
发明目的：本发明的目的是提供一种膜/基结合强度高、服役寿命长的钛合金表面共掺杂抗菌/骨诱导材料。
技术方案：本发明的钛合金表面共掺杂抗菌/骨诱导材料，所述材料包括具有微孔结构的钛合金基体，覆盖在钛合金基底表面的原位成形Ag-N-HA共掺杂TiO2膜层。
一种上述钛合金表面共掺杂抗菌/骨诱导材料的制备方法，包括以下步骤：
(1)钛合金分别置于丙酮、无水乙醇中超声清洗；
(2)在水中加入硝酸银和纳米羟基磷灰石并混合均匀，所得的混合溶液经压力雾化器喷洒于步骤(1)中清洗后的钛合金的表面上；
(3)在氮气气氛下，使用飞秒激光在钛合金的表面上扫描加工，得到钛合金表面共掺杂抗菌/骨诱导材料。
进一步地，所述步骤(1)中钛合金为医用纯钛或TC4合金。
进一步地，所述步骤(2)中硝酸银的浓度为0.2～1mol/L，纳米羟基磷灰石的浓度为0.5～2g/L。
进一步地，所述步骤(2)中压力雾化器的移动速率为50～500mm/s。
进一步地，所述步骤(3)中飞秒激光的脉冲功率为0.5～1.5W。
发明原理：依据钛合金骨植入体抗菌及骨诱导功能需求，基于TiO2的电子结构及形成特性，采用将含Ag离子及纳米HA粒子的混合溶液通过压力雾化器喷洒于钛合金表面，根据飞秒激光能量特点及对N/Ti/Ag间的热力耦合作用，在钛合金表面原位成形Ag-N-HA共掺杂TiO2微孔结构。该原位结构与钛合金基体结合强度高，同时所掺杂的Ag离子与纳米HA能共同发挥其抗菌和骨诱导功能；另一方面钛合金表面的高比面积微孔结构与人体组织间具有较强的机械嵌合能力，增强钛合金植入体与周围组织的嵌骨结合强度，提高钛合金的综合服役性能和使用寿命。
有益效果：与现有技术相比，本发明具有如下显著优点：(1)膜/基结合强度高，在钛合金表面采用氮气/雾化辅助一步法激光原位成形具有Ag-N-HA共掺杂TiO2微孔结构，能增强其与钛合金基体的膜/基结合强度，有效延长钛合金植入体的服役寿命；
(2)制备工艺简单，基于钛合金骨植入体的生物功能需求，采用雾化将含Ag离子及纳米HA粒子的混合溶液通过压力雾化器喷洒于钛合金表面，利用氮气辅助一步法激光原位成形Ag-N-HA共掺杂TiO2微孔结构；另一方面通过混合溶液雾化速率的控制，实现Ag与HA掺杂量的改变。
(3)具有抗菌功能，微米尺度的Ag-N-HA共掺杂TiO2微孔结构为钛合金植入体周围组织向孔隙内生长提供了通道，同时HA诱导骨组织的生长，促进钛合金与骨组织间形成纤维组织膜，形成机械嵌合，实现了微结构/功能的一体化制造。
附图说明
图1为实施例1中制造的钛合金表面共掺杂抗菌/骨诱导微孔结构的显微形貌图；
图2为实施例2中制造的钛合金表面共掺杂抗菌/骨诱导微孔结构的成分谱图；
图3为实施例1-4中制造的钛合金表面共掺杂抗菌/骨诱导微孔结构的抗菌性能对比图。
具体实施方式
实施例1
(1)将医用纯钛分别在丙酮、无水乙醇中超声清洗15min；
(2)将0.2mol/L硝酸银与0.5g/L纳米羟基磷灰石HA加入到100ml超纯水中超声分数形成混合溶后，经压力雾化器按500mm/s速率喷洒于步骤(1)中所述的医用纯钛表面；
(3)在氮气气氛保护下，借助飞秒激光的脉冲功率为0.5W在步骤(2)所述医用纯钛表面扫描加工，成形原位Ag-N-HA共掺杂TiO2微孔结构。
实施例2
(1)将医用TC4分别在丙酮、无水乙醇中超声清洗15min；
(2)将0.6mol/L硝酸银与1g/L纳米羟基磷灰石HA加入到100ml超纯水中超声分数形成混合溶后，经压力雾化器按250mm/s速率喷洒于步骤(1)中所述的医用TC4表面；
(3)在氮气气氛保护下，借助飞秒激光的脉冲功率为1W在步骤(2)所述医用TC4表面扫描加工，成形原位Ag-N-HA共掺杂TiO2微孔结构。
实施例3
(1)将医用纯钛分别在丙酮、无水乙醇中超声清洗15min；
(2)将0.8mol/L硝酸银与1g/L纳米羟基磷灰石HA加入到100ml超纯水中超声分数形成混合溶后，经压力雾化器按200mm/s速率喷洒于步骤(1)中所述的医用纯钛表面；
(3)在氮气气氛保护下，借助飞秒激光的脉冲功率为1W在步骤(2)所述医用纯钛表面扫描加工，成形原位Ag-N-HA共掺杂TiO2微孔结构。
实施例4
(1)将医用纯钛分别在丙酮、无水乙醇中超声清洗15min；
(2)将1mol/L硝酸银与2g/L纳米羟基磷灰石HA加入到100ml超纯水中超声分数形成混合溶后，经压力雾化器按50mm/s速率喷洒于步骤(1)中所述的医用纯钛表面；
(3)在氮气气氛保护下，借助飞秒激光的脉冲功率为1.5W在步骤(2)所述医用纯钛表面扫描加工，成形原位Ag-N-HA共掺杂TiO2微孔结构。
实施例2、3和4中制造的钛合金表面共掺杂抗菌/骨诱导微孔结构的对金黄色葡萄球菌在试验24h后的抑菌率均在99.9％，高于单一Ag掺杂钛合金的抑菌率(99.5％)，具有良好的抗菌功能。
如图1所示为上述实施例1中制造的钛合金表面共掺杂抗菌/骨诱导微孔结构的显微结构图。图2为实施例2中制造的钛合金表面共掺杂抗菌/骨诱导微孔结构的成分谱图。从上图中可发现，在钛合金表面微孔结构多呈椭圆形或近圆形，结合图2谱图，其表面存在白色纳米颗粒状的HA，且其中含有掺杂N元素的Ag离子，说明本本发明提供的方法可一步法激光原位成形具有Ag-N-HA共掺杂TiO2微孔结构。为进一步证明本发明制备的Ag-N-HA共掺杂TiO2微孔结构的抗菌功能，对其抗菌性能进行评价，以证明本发明的技术优势。图3为实施例1-4中制造的钛合金表面共掺杂抗菌/骨诱导微孔结构的抗菌性能对比图，一方面通过合理调控负载Ag+-N-羟基磷灰石纳米粉体所占复合粉体的质量比，可增强功能性植入体的抗菌功能；另一方面可以发现对金黄色葡萄球菌在试验24h后的抑菌率均在98.1％，高于单一Ag/HA掺杂钛合金的抑菌率(92.47％)，具有良好的抗菌功能。

Claims (5)

1.一种钛合金表面共掺杂抗菌/骨诱导材料的制备方法，其特征在于，包括以下步骤：
（1）钛合金分别置于丙酮、无水乙醇中超声清洗；
（2）在水中加入硝酸银和纳米羟基磷灰石并混合均匀，所得的混合溶液经压力雾化器喷洒于步骤（1）中清洗后的钛合金的表面上；
（3）在氮气气氛下，使用飞秒激光在钛合金的表面上扫描加工，得到钛合金表面共掺杂抗菌/骨诱导材料，所述材料包括具有微孔结构的钛合金基体，覆盖在钛合金基底表面的原位成形Ag-N-HA共掺杂TiO2膜层。
2.根据权利要求1所述的钛合金表面共掺杂抗菌/骨诱导材料的制备方法，其特征在于，所述步骤（1）中钛合金为医用纯钛或TC4合金。
3.根据权利要求1所述的钛合金表面共掺杂抗菌/骨诱导材料的制备方法，其特征在于，所述步骤（2）中硝酸银的浓度为0.2～1 mol/L，纳米羟基磷灰石的浓度为0.5～2 g/L。
4.根据权利要求1所述的钛合金表面共掺杂抗菌/骨诱导材料的制备方法，其特征在于，所述步骤（2）中压力雾化器的移动速率为50～500 mm/s。
5.根据权利要求1所述的钛合金表面共掺杂抗菌/骨诱导材料的制备方法，其特征在于，所述步骤（3）中飞秒激光的脉冲功率为0.5～1.5 W。
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