CN115177791A - 一种生物相容性好的MXenes生物涂层的制备及其应用 - Google Patents
一种生物相容性好的MXenes生物涂层的制备及其应用 Download PDFInfo
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Abstract
本发明提供了一种生物相容性好的生物涂层及其制备方法,其中,所述的生物涂层用作为医用金属、医用合金、医用无机非金属材料、医用高分子材料的基材的表面,其为钛系、锂系及钒系的MXenes材料。本发明的生物涂层不仅具有优良的生物活性和生物相容性,还具有优异的抗菌性,因此可广泛应用于植入生物材料领域。
Description
技术领域
本发明涉及医用涂层技术邻域,具体涉及一种生物相容性好的MXenes生物涂层的制备及其应用。
背景技术
植入体感染是植入体手术术后严重并发症之一,难以预防。虽然手术前,医生做了各种预防细菌污染的手术准备,但术后感染仍旧不能避免。为减少术后感染的发生,近几十年来,人们在无菌技术、无菌环境及手术期预防性应用抗生素方面的研究取得重大进展,抗菌植入体材料成为减少术后感染的有效手段被应用于医疗领域。对植入体表面进行涂层修饰提高其表面的抗菌性成为研究热点。
抗菌涂层是指以植入体材料为基体,通过喷涂、溶胶-凝胶、复合镀、离子注入、磁控溅射等工艺将具有抗菌功能的各种材料涂覆在基体上。由于抗菌涂层随着应用会逐渐被磨耗,无法维持长期的抗菌功效,所以如何增强抗菌涂层与基体的结合力,并获得良好的抗菌性、生物相容性、高耐磨性是目前研究的关键问题。
MXenes是一类具有Mn+1XnTx元素构成的材料体系,其中M表示早期过渡族金属元素,X表示C或者N,T指的是该二维材料表面的基团/修饰体,n通常取值范围为1-3。因此,MXene家族拥有丰富的化学构成,成员众多,并且还在不断扩张。MXenes具有优异的电学性能和光学性能,在能源存储和电磁方面有诸多的应用。近些年来,MXene材料在生物领域的应用被不断开发。
目前,多项研究报道了MXenes材料的抗菌性。Mahmoud等人的研究表明,Ti3C2Tx,一种典型的MXenes材料,对革兰氏阴性的大肠杆菌和革兰氏阳性的枯草杆菌均有抗菌作用,其抗菌活性呈剂量依赖性且抗菌效率高于氧化石墨烯。与石墨烯类似,Ti3C2Tx通过破坏细胞膜和产生活性氧(ROS)来抑制细菌。然而,有些细菌可以通过能够通过产生抗氧化剂来抵制基于氧化剂的清除机制。因此,涉及氧化应激的抗菌机制可能对这些细菌的效果欠佳甚至无效。利用MXenes材料高的光热转化效率,洪伟礼等人使用光热治疗(PPT)协同抗菌。Ti3C2 MXenes在近红外光照射下通过光热效应快速的杀灭细菌,对15种检测细菌(包括革兰氏阳性菌、革兰氏阴性菌、抗生素耐药菌)均有效,具有广谱的抗菌作用。其次,MXene材料具有优异的生物相容性,在小鼠体内治疗实验中未显示出明显的毒副作用。此外,MXenes材料在药物递送方面也存在巨大的潜力,通过负载药物达到协同抗菌或治疗的作用。
发明内容
本发明制备了一种生物相容性好的MXenes生物涂层,该MXenes生物涂层通过滴涂、喷涂、浸涂的方式涂覆在基体上,其具有优良的生物相容性和抗菌性,MXenes生物涂层的制备方法如下:
MXenes二维纳米材料可通过盐酸/氟化锂刻蚀法制备,具体包括以下步骤:
步骤一:MXenes二维材料制备:在室温条件下,将1g 氟化锂(LiF)溶于20mL 盐酸(HCl)中(V浓HCl:VH2O=1:1),制备LiF/HCl的混合物。将1g MAX相前驱体的浸入20 mL LiF/HCl溶液中,在室温下搅拌反应72 h,得到多层的MXenes。蚀刻后,用去离子水洗涤得到的悬浮液,并离心将粉末从上清液中分离出来。 经几次洗涤后,使pH大于6,并真空干燥。
其中,所述MAX相前驱体是一类化学通式为Mn+1AXn的三元层状化合物,其中M是早期过渡金属,例如Ti,Li,V,Zn,Ga,Ge,Cr等;A是Ⅲ、Ⅳ主族元素,X是C或N,n代表1,2,3等。
步骤二:在多层MXens中加入去离子水使其分散,超声2h后,抽滤悬浮液,得到的悬浮液即为MXenes溶液。
步骤三:将基体材料分别用去离子水、无水乙醇超声清洗,去除表面的油脂和杂质,在真空干燥箱中干燥。
步骤四:将步骤三中得到的基体材料进行表面喷砂处理,然后在氩气的保护下,将MXenes通过喷涂、浸涂、滴涂的方法涂覆在基体材料上。
含钒的MXene二维纳米材料可通过氟化氢刻蚀法制备,具体包括以下步骤:
步骤一:含钒MXene二维材料制备:将1g MAX相前驱体的浸入10 mL HF溶液(55wt.%)中,35℃搅拌反应92 h,得到多层的MXenes。蚀刻后,用去离子水洗涤得到的悬浮液,并离心将粉末从上清液中分离出来。 经几次洗涤后,使pH大于6,并真空干燥。
其中,所述MAX相前驱体是一类化学通式为Mn+1AXn的三元层状化合物,其中M是早期过渡金属,例如Ti,Li,V,Zn,Ga,Ge,Cr等;A是Ⅲ、Ⅳ主族元素,X是C或N,n代表1,2,3等。
步骤二:将1g步骤一制备的多层MXenes加入到10mL插层剂四丁基氢氧化铵(TBA-OH)中,搅拌24h后,使用真空抽滤装置抽滤,去除插层MXenes,用去离子水抽滤清洗至pH大于6,置于真空干燥箱中在60℃下干燥24小时后得到的固体粉末即为单层的MXenes基纳米材料。
步骤三:将基体材料分别用去离子水、无水乙醇超声清洗,去除表面的油脂和杂质,在真空干燥箱中干燥。
步骤四:将步骤三中得到的基体材料进行表面喷砂处理,然后在氩气的保护下,将MXenes通过喷涂、浸涂、滴涂的方法涂覆在基体材料上。
附图说明
图1是本发明一个实施案例中使用MXenes生物涂层喷涂的心脏支架示意图。
图2是本发明一个实施案例中使用MXenes生物涂层喷涂的鼻梁填充硅胶假体示意图。
图3是本发明一个实施案例中的钒系MXenes生物涂层对大肠杆菌的抗菌效果图。
具体实施方法
在下文中,将通过具体的实施例更加详细的描述本发明,但所提供的实施例仅是说明性的,并不意欲限制本发明。
实施例1:
(1)将10 mL去离子水、10 mL浓度为12M的盐酸和1g氟化锂混合到容量为60mL的高密度聚乙烯瓶中,搅拌并加热到35℃。随后加入1g由Ti3AlC2相前驱体,搅拌72小时后,用去离子水抽滤清洗至pH大于6,将得到的沉淀物置于真空干燥箱中在60℃下干燥24小时;
(2)将多层Ti3C2沉淀物分散到100mL去离子水中,超声2h后,使用真空抽滤装置抽滤,去除插层Ti3C2,抽滤瓶中的悬浮液即为单层的Ti3C2基纳米材料;
(3)将合金基材分别用去离子水、无水乙醇超声清洗,去除表面的油脂和杂质,在真空干燥箱中干燥;
(4)将步骤三中得到的合金基材进行表面喷砂处理,然后在氩气的保护下,将Ti3C2溶液通过喷涂的方法涂覆在基体材料上。
实施例2:
(1)将10 mL去离子水、10 mL浓度为12M的盐酸和1g氟化锂混合到容量为60mL的高密度聚乙烯瓶中,搅拌并加热到35℃。随后加入1g由Ti3AlC2相前驱体,搅拌72小时后,用去离子水抽滤清洗至pH大于6,将得到的沉淀物置于真空干燥箱中在60℃下干燥24小时;
(2)将多层Ti3C2沉淀物分散到100mL去离子水中,超声2h后,使用真空抽滤装置抽滤,去除插层Ti3C2,抽滤瓶中的悬浮液即为单层的Ti3C2基纳米材料;
(3)将医用硅胶分别用去离子水、无水乙醇超声清洗,去除表面的油脂和杂质,在真空干燥箱中干燥;
(4)在氩气的保护下,将Ti3C2溶液通过滴涂的方法涂覆在医用硅胶上。
实施例3:
(1)将10 mL去离子水、10 mL浓度为12M的盐酸和1g氟化锂混合到容量为60mL的高密度聚乙烯瓶中,搅拌并加热到35℃。随后加入1g由Ti3AlC2相前驱体,搅拌72小时后,用去离子水抽滤清洗至pH大于6,将得到的沉淀物置于真空干燥箱中在60℃下干燥24小时;
(2)将多层Ti3C2沉淀物分散到100mL去离子水中,超声2h后,使用真空抽滤装置抽滤,去除插层Ti3C2,抽滤瓶中的悬浮液即为单层的Ti3C2基纳米材料;
(3)将羟基磷灰石分别用去离子水、无水乙醇超声清洗,去除表面的油脂和杂质,在真空干燥箱中干燥;
(4)将步骤三中得到的羟基磷灰石进行表面喷砂处理,然后在氩气的保护下,将Ti3C2溶液通过喷涂的方法涂覆在羟基磷灰石上。
实施例4:
(1)将10 mL去离子水、10 mL浓度为12M的盐酸和1g氟化锂混合到容量为60mL的高密度聚乙烯瓶中,搅拌并加热到35℃。随后加入1g由Ti3AlC2相前驱体,搅拌72小时后,用去离子水抽滤清洗至pH大于6,将得到的沉淀物置于真空干燥箱中在60℃下干燥24小时;
(2)将多层Ti3C2沉淀物分散到100mL去离子水中,超声2h后,使用真空抽滤装置抽滤,去除插层Ti3C2,抽滤瓶中的悬浮液即为单层的Ti3C2基纳米材料;
(3)将聚乳酸分别用去离子水、无水乙醇超声清洗,去除表面的油脂和杂质,在真空干燥箱中干燥;
(4)将步骤三中得到的聚乳酸进行表面喷砂处理,然后在氩气的保护下,将Ti3C2溶液通过喷涂的方法涂覆在聚乳酸基材上。
实施例5:
(1)将10 mL去离子水、10 mL浓度为12M的盐酸和1g氟化锂混合到容量为60mL的高密度聚乙烯瓶中,搅拌并加热到35℃。随后加入1g由TiVAlC相前驱体,搅拌72小时后,用去离子水抽滤清洗至pH大于6,将得到的沉淀物置于真空干燥箱中在60℃下干燥24小时;
(2)将多层TiVC沉淀物分散到100mL去离子水中,超声2h后,使用真空抽滤装置抽滤,去除插层TiVC,抽滤瓶中的悬浮液即为单层的TiVC基纳米材料;
(3)将合金基材分别用去离子水、无水乙醇超声清洗,去除表面的油脂和杂质,在真空干燥箱中干燥;
(4)将步骤三中得到的合金基材进行表面喷砂处理,然后在氩气的保护下,将TiVC溶液通过喷涂的方法涂覆在合金基材上。
实施例6:
(1)将10 mL去离子水、10 mL浓度为12M的盐酸和1g氟化锂混合到容量为60mL的高密度聚乙烯瓶中,搅拌并加热到35℃。随后加入1g由TiVAlC相前驱体,搅拌72小时后,用去离子水抽滤清洗至pH大于6,将得到的沉淀物置于真空干燥箱中在60℃下干燥24小时;
(2)将多层TiVC沉淀物分散到100mL去离子水中,超声2h后,使用真空抽滤装置抽滤,去除插层TiVC,抽滤瓶中的悬浮液即为单层的TiVC基纳米材料;
(3)将医用硅胶分别用去离子水、无水乙醇超声清洗,去除表面的油脂和杂质,在真空干燥箱中干燥;
(4)在氩气的保护下,将TiVC溶液通过滴涂的方法涂覆在医用硅胶上。
实施例7:
(1)将10 mL去离子水、10 mL浓度为12M的盐酸和1g氟化锂混合到容量为60mL的高密度聚乙烯瓶中,搅拌并加热到35℃。随后加入1g由TiVAlC相前驱体,搅拌72小时后,用去离子水抽滤清洗至pH大于6,将得到的沉淀物置于真空干燥箱中在60℃下干燥24小时;
(2)将多层TiVC沉淀物分散到100mL去离子水中,超声2h后,使用真空抽滤装置抽滤,去除插层TiVC,抽滤瓶中的悬浮液即为单层的TiVC基纳米材料;
(3)将羟基磷灰石分别用去离子水、无水乙醇超声清洗,去除表面的油脂和杂质,在真空干燥箱中干燥;
(4)将步骤三中得到的羟基磷灰石进行表面喷砂处理,然后在氩气的保护下,将TiVC溶液通过喷涂的方法涂覆在羟基磷灰石上。
实施例8:
(1)将10 mL去离子水、10 mL浓度为12M的盐酸和1g氟化锂混合到容量为60mL的高密度聚乙烯瓶中,搅拌并加热到35℃。随后加入1g由TiVAlC相前驱体,搅拌72小时后,用去离子水抽滤清洗至pH大于6,将得到的沉淀物置于真空干燥箱中在60℃下干燥24小时;
(2)将多层TiVC沉淀物分散到100mL去离子水中,超声2h后,使用真空抽滤装置抽滤,去除插层TiVC,抽滤瓶中的悬浮液即为单层的TiVC基纳米材料;
(3)将聚乳酸分别用去离子水、无水乙醇超声清洗,去除表面的油脂和杂质,在真空干燥箱中干燥;
(4)将步骤三中得到的聚乳酸进行表面喷砂处理,然后在氩气的保护下,将TiVC溶液通过喷涂的方法涂覆在聚乳酸基材上。
Claims (7)
1.一种生物相容性好的MXenes生物涂层的制备,其特征在于,所述的MXenes生物涂层包括但不限于锂系、钛系、钒系的MXenes材料及其复合物。
2.根据权利要求一所述的一种生物相容性好的MXenes生物涂层的制备,其特征在于,所述的MXenes材料包括但不限于单层MXenes材料、多层MXenes材料、MXenes 量子点及上述材料的复合物。
3.根据权利要求一和要求二所述的一种生物相容性好的MXenes生物涂层的制备,其特征在于,所述的Mxenes生物涂层包括但不限于MXenes涂层以及载药的MXenes涂层。
4.根据权利要求三所述的一种生物相容性好的MXenes生物涂层的制备,其特征在于,是在金属及其合金、无机非金属材料及复合物、高分子材料及复合物基材的表面形成的涂层;其中,所述的金属及其合材料包括但不限于不锈钢材料、钛及钛合金、铝及铝合金;所述的无机非金属材料及复合物包括但不限于硅胶、羟基磷灰石、陶瓷;所述的高分子材料及复合物包括但不限于聚乳酸、聚醚醚酮、聚乳酸-羟基乙酸共聚物。
5.根据权利要求四所述的一种生物相容性好的MXenes生物涂层的制备,其特征在于,采用喷涂、浸涂、滴涂的方法在基材表面形成涂层。
6.根据权利要求五所述一种生物相容性好的MXenes生物涂层的制备,其特征在于,基材表面的涂层厚度为0.001-1000μm。
7.根据权利要求一至权利要求六所述的一种生物相容性好的MXenes生物涂层的制备,其特征在于,所制备的MXenes生物涂层的应用包括但不限于Mxenes涂覆的医用支架、Mxenes涂覆的医用假体、Mxenes涂覆的口腔种植体、Mxenes涂覆的骨科植入体。
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