CN115054726A - 一种近红外响应抗菌骨修复材料及其制备方法与应用 - Google Patents
一种近红外响应抗菌骨修复材料及其制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种近红外响应抗菌骨修复材料及其制备方法与应用。所述方法为:利用激光对钛基金属材料表面进行微区烧蚀处理,由于激光束的高温熔融淬火及激光束扫描区域重叠,可在钛基材料表面原位构建具有微纳米多级结构的黑色氧化钛结构。所得到的钛基材料微纳米多级结构的黑色氧化钛表面可在近红外光作用下产生光热效应杀灭细菌,且具有良好的生物相容性。
Description
技术领域
本发明属于生物医用材料技术领域,具体涉及一种近红外响应抗菌骨修复材料及其制备方法与应用。
背景技术
钛合金强度高、耐腐蚀性和生物相容性优异,广泛用于从骨折固定到畸形矫正等骨科应用中。然而,钛合金材料易受细菌感染,导致并发症甚至固定失败,危及患者生命安全。为解决术后感染问题,临床上对患者的治疗往往依赖于长期使用抗生素和多次手术清创,导致多重耐药菌的产生和传播,给患者带来痛苦和沉重的负担。因此,开发非侵入性、高效、可远程控制的非抗生素的抗菌策略已迫在眉睫。
近红外光响应光热疗法(NIR-PTT)是一种很有前途的抗菌策略,它利用光热材料吸收和转换NIR光为热能以高温杀灭细菌。由于近红外光具有较高的组织穿透深度和对生物体内血液和水的吸收率低,近红外光PTT由于其无创和远程可控的治疗方式,精确的时空可控性,近年来引起了人们的广泛关注。虽然近红外响应光热剂(石墨烯,二硫化钼和光敏剂等)被用于修饰钛合金表面以获得NIR-PTT抗菌性能,但生物安全性和结构稳定性限制了它们的光热功效和临床应用。目前,尚缺乏具有令人满意的生物相容性、高结构稳定性的光热转换材料。
发明内容
为解决现有技术的缺点和不足之处,本发明的首要目的在于提供一种近红外响应抗菌骨修复材料的制备方法,简单高效地在钛基材料表面原位构建微纳米多级结构的黑色氧化钛材料。
本发明的另一目的在于提供上述方法制得的一种近红外响应抗菌骨修复材料。
本发明利用脉冲激光烧蚀处理在钛基材料表面原位构建具有多级结构的黑色氧化钛层,可有效利用近红外光进行光热抗菌应用。此外,黑色氧化钛植入材料生物相容性好,结构稳定,可实现近红外光驱动的非侵入性、高效、可远程控制的非抗生素的骨科手术后临床感染治疗。
本发明的再一目的在于提供上述一种近红外响应抗菌骨修复材料的应用。
本发明目的通过以下技术方案实现:
一种近红外响应抗菌骨修复材料的制备方法,包括以下步骤:
利用脉冲激光对钛基金属材料表面进行微区烧蚀处理,其中激光功率为5~20W,扫描速度为10~500mm/s,扫描间距为0~30μm,扫描间距小于激光束斑直径,得到钛基材料表面具有微纳米多级结构的黑色氧化钛材料。
优选地,所述激光束斑直径为1~100μm。
优选地,所述钛基金属材料为TA3、TA4和TC4中的一种。
所述扫描间距指激光移动路径的两条相对直线或曲线间的距离,这两条相对直线或曲线的间距相较于激光在金属表面形成的束斑直径要小,使得激光可以对同一位置进行重复烧蚀氧化。
优选地,所述激光功率为8~20W,扫描速度为100~300mm/s,扫描间距为10~20μm。
更优选地,所述激光束斑直径为30μm,激光功率为8W,激光扫描速度为100mm/s,扫描间距为10μm。
优选地,所述脉冲激光发生器为光纤激光器、气体激光器、固体激光器或半导体激光器。
优选地,所述钛基金属材料在微区烧蚀处理前,利用丙酮、无水乙醇和去离子水清洗并干燥。
上述方法制得的一种近红外响应抗菌骨修复材料。
所述近红外响应抗菌骨修复材料,其钛基材料表面具有微纳米多级结构的黑色氧化钛表面,可在近红外光作用下产生光热效应杀灭细菌。
上述一种近红外响应抗菌骨修复材料在医疗器械加工领域的应用。
本发明采用脉冲激光烧蚀处理在钛基材料表面开发出具有优异生物相容性和近红外响应特性的黑色氧化钛,不引入其他有毒元素或化合物。具有微/纳米多级结构的黑色氧化钛可有效利用近红外光进行光热抗菌应用,有利于防治骨科手术后植入材料周围感染。
与现有技术相比,本发明具有以下优点及有益效果:
本发明利用激光原位烧蚀氧化构建具有微纳米多级结构的黑色氧化钛表面用于近红外驱动的光热抗菌,具有良好生物相容性、高结构稳定性和优异光热转换能力的近红外光热响应钛基植入材料。本发明制备方法简单、高效,可应用于各类钛基骨修复材料的表面抗菌功能化处理,临床意义重大。
附图说明
图1为激光烧蚀钛基金属表面原位生长微纳米多级结构黑色氧化钛的表面形貌及成分组成图。(a)为对比例1中低功率(3W)处理钛和实施例1中微纳米多级结构黑色氧化钛的光学照片。(b)和(c)分别为实施例1中微纳米多级结构黑色氧化钛的扫描电镜图和微纳米多级结构黑色氧化钛的XPS全谱图。
图2为实施例1微区激光处理后所得TC4钛合金材料在体外的吸收光谱和光热效应。(a)为对比例1中低功率处理钛和实施例1中微纳米多级结构黑色氧化钛的UV-Vis-NIR吸收光谱;(b)为在808nm NIR照射(10min,1.0W/cm2)下、磷酸盐缓冲盐水(PBS)溶液中测量的对比例1中低功率处理钛和实施例1中微纳米多级结构黑色氧化钛的光热成像仪图像;(c)为实施例1中微纳米多级结构黑色氧化钛的在连续808nm近红外激光照射(10min,1.0W/cm2)下五个开关循环的温度上升和下降。
图3为平板菌落计数实验。(a)在体外不同组金黄色葡萄球菌的琼脂板菌落计数照片。(b)表示对比例1中低功率处理钛和实施例1中微纳米多级结构黑色氧化钛组在808nm近红外光照(10min,1.0W/cm2)和黑暗条件下的抗菌效率。(c)不同组材料表面金黄色葡萄球菌的扫描电镜图。(d)不同组材料表面金黄色葡萄球菌的死活细菌染色荧光图。
图4为不同组材料的体外小鼠骨髓间充质干细胞增殖试验和溶血试验评价。(a)为对比例1中低功率处理钛和实施例1中微纳米多级结构黑色氧化钛组材料表面细胞的CCK-8检测。(b)为与样品共培养的全血中提取的血清照片和相应的溶血率值。
图5为实施例2-5以及对比例2条件下激光处理得到材料的光学图片。
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。
本发明实施例中未注明具体条件者,按照常规条件或者制造商建议的条件进行。所用未注明生产厂商者的原料、试剂等,均为可以通过市售购买获得的常规产品。
实施例1
一种近红外响应抗菌骨修复材料的制备方法,包括以下步骤:
依次利用丙酮、无水乙醇和去离子水清洗TC4钛合金材料并真空干燥;
对光纤激光器进行聚焦,使用光纤激光器对TC4钛合金材料进行微区激光处理,引发激光烧蚀重叠微区的熔融氧化以构建近红外响应抗菌骨修复材料。其中激光束斑直径30μm,激光烧蚀功率为8W,激光扫描速度为100mm/s,扫描间距为10μm,扫描路径为直线。
本实施例微区激光处理后所得TC4钛合金材料的光学照片及表面扫描电镜形貌如图所示,其中(a)为TC4钛合金激光诱导微纳米多级结构黑色氧化钛的光学照片;(b)和(c)为不同倍数的TC4钛合金激光诱导微纳米多级结构黑色氧化钛的扫描电镜图和X射线光电子能谱图。利用激光对钛基金属材料表面进行微区烧蚀处理,由于激光束的高温熔融淬火及激光束扫描区域重叠,所得到的钛基材料表面具有微纳米多级结构的黑色氧化钛表面。
本实施例微区激光处理后所得TC4钛合金材料在近红外光照射下的光热效应如图2所示,所得到的钛基材料表面微纳米多级结构的黑色氧化钛具有良好的光热效应。
本实施例微区激光处理后所得TC4钛合金材料在近红外光照射下的光热抗菌效果如图3所示,所得到的钛基材料表面微纳米多级结构的黑色氧化钛可在近红外光作用下产生光热效应杀灭细菌。
本实施例微区激光处理后所得TC4钛合金材料的生物安全性评价如图4所示,该微纳米多级结构的黑色氧化钛具有良好的细胞相容性和血液相容性。
实施例2
一种近红外响应抗菌骨修复材料的制备方法,包括以下步骤:
依次利用丙酮、无水乙醇和去离子水清洗TA4纯钛材料并真空干燥;
对光纤激光器进行聚焦,使用光纤激光器对TA4纯钛材料进行微区激光处理,引发激光烧蚀重叠微区的熔融氧化以构建近红外响应抗菌骨修复材料。其中激光束斑直径30μm,激光烧蚀的功率为15W,激光扫描速度为300mm/s,扫描间距为10μm,扫描路径为直线,得到微纳米多级结构黑色氧化钛表面,其光学图片如图5所示。
实施例3
一种近红外响应抗菌骨修复材料的制备方法,包括以下步骤:
依次利用丙酮、无水乙醇和去离子水清洗TC4钛合金材料并真空干燥;
对半导体激光器进行聚焦,使用半导体激光器对TC4钛合金材料进行微区激光处理,引发激光烧蚀重叠微区的熔融氧化以构建近红外响应抗菌骨修复材料。其中激光束斑直径30μm,激光烧蚀的功率为20W,激光扫描速度为100mm/s,扫描间距为10μm,扫描路径为直线,该条件下仍能得到微纳米多级结构黑色氧化钛表面,其光学图片如图5所示。
实施例4
一种近红外响应抗菌骨修复材料的制备方法,包括以下步骤:
依次利用丙酮、无水乙醇和去离子水清洗TC4钛合金材料并真空干燥;
对光纤激光器进行聚焦,使用光纤激光器对TC4钛合金材料进行微区激光处理,引发激光烧蚀重叠微区的熔融氧化以构建近红外响应抗菌骨修复材料。其中激光束斑直径30μm,激光烧蚀的功率为8W,激光扫描速度为100mm/s,扫描间距为10μm,扫描路径为同心圆弧,得到微纳米多级结构黑色氧化钛表面,其光学图片如图5所示。
实施例5
一种近红外响应抗菌骨修复材料的制备方法,包括以下步骤:
依次利用丙酮、无水乙醇和去离子水清洗TC4钛合金材料并真空干燥;
对光纤激光器进行聚焦,使用光纤激光器对TC4钛合金材料进行微区激光处理,引发激光烧蚀重叠微区的熔融氧化以构建近红外响应抗菌骨修复材料。其中激光束斑直径30μm,激光烧蚀的功率为8W,激光扫描速度为100mm/s,扫描间距为20μm,扫描路径为直线,得到微纳米多级结构黑色氧化钛表面,其光学图片如图5所示。
对比例1
依次利用丙酮、无水乙醇和去离子水清洗TC4钛合金材料并真空干燥;
对光纤激光器进行聚焦,使用光纤激光器对TC4钛合金材料进行微区激光处理,引发激光烧蚀重叠微区的熔融氧化以构建近红外响应抗菌骨修复材料。其中激光束斑直径30μm,激光烧蚀的功率条件为3W,激光扫描速度为100mm/s,扫描间距为10μm,扫描路径为直线。该条件下不能得到黑色氧化钛表面,如图1所示。
对比例2
依次利用丙酮、无水乙醇和去离子水清洗TC4钛合金材料并真空干燥;
对光纤激光器进行聚焦,使用光纤激光器对TC4钛合金材料进行微区激光处理,引发激光烧蚀重叠微区的熔融氧化以构建近红外响应抗菌骨修复材料。其中激光束斑直径30μm,激光烧蚀的功率条件为8W,激光扫描速度为100mm/s,扫描间距为50μm(大于激光束斑直径),扫描路径为直线。该条件下处理得到浅灰色表面(如图5所示),近红外光热性能低于实施例中微纳米多级结构黑色氧化钛材料表面。
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)
1.一种近红外响应抗菌骨修复材料的制备方法,其特征在于,包括以下步骤:
利用脉冲激光对钛基金属材料表面进行微区烧蚀处理,其中激光功率为5~20W,扫描速度为10~500mm/s,扫描间距为0~30μm,扫描间距小于激光束斑直径,得到钛基材料表面具有微纳米多级结构的黑色氧化钛材料。
2.根据权利要求1所述一种近红外响应抗菌骨修复材料的制备方法,其特征在于,所述激光束斑直径为1~100μm。
3.根据权利要求1所述一种近红外响应抗菌骨修复材料的制备方法,其特征在于,所述激光功率为8~20W,扫描速度为100~300mm/s,扫描间距为10~20μm。
4.根据权利要求2所述一种近红外响应抗菌骨修复材料的制备方法,其特征在于,所述激光束斑直径为30μm。
5.根据权利要求1所述一种近红外响应抗菌骨修复材料的制备方法,其特征在于,所述激光束斑直径为30μm,激光功率为8W,激光扫描速度为100mm/s,扫描间距为10μm。
6.根据权利要求1所述一种近红外响应抗菌骨修复材料的制备方法,其特征在于,所述钛基金属材料为TA3、TA4和TC4中的一种。
7.根据权利要求1所述一种近红外响应抗菌骨修复材料的制备方法,其特征在于,所述脉冲激光发生器为光纤激光器、气体激光器、固体激光器或半导体激光器。
8.根据权利要求1所述一种近红外响应抗菌骨修复材料的制备方法,其特征在于,所述钛基金属材料在微区烧蚀处理前,利用丙酮、无水乙醇和去离子水清洗并干燥。
9.权利要求1~8任一项所述制备方法制得的一种近红外响应抗菌骨修复材料。
10.权利要求9所述一种近红外响应抗菌骨修复材料在医疗器械加工领域的应用。
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