CN117100906A - 一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的制备方法及应用 - Google Patents
一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的制备方法及应用 Download PDFInfo
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- CN117100906A CN117100906A CN202311133356.8A CN202311133356A CN117100906A CN 117100906 A CN117100906 A CN 117100906A CN 202311133356 A CN202311133356 A CN 202311133356A CN 117100906 A CN117100906 A CN 117100906A
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Abstract
一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的制备方法及应用,经过合成中空介孔二氧化硅纳米颗粒,并将其涂覆于多孔钛合金植入物表面,形成一种纳米结构涂层;将构建了HMSNs涂层的多孔钛合金植入物置于双磷酸盐溶液中,在室温条件下振荡12‑48h,完成双磷酸盐的负载;HMSNs能够均匀分布在多孔钛合金植入物表面及内部小梁结构,有利于细胞附着,提高了多孔钛合金植入物的生物活性;HMSNs涂层能够吸附并缓释双磷酸盐,具有调控植入物周围微环境成骨‑破骨平衡的生物功能。
Description
技术领域
本发明属于生物医用材料多孔钛合金植入物的表面改性领域,特别涉及一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的制备方法及应用。
背景技术
骨质疏松症(Osteoporosis, OP)是骨科最常见的全身性疾病之一,以骨量减低、骨的微结构破坏、骨脆性增加为主要特征。临床病例回顾分析显示,OP患者关节置换术后,假体下沉和假体松动、假体周围骨折的发生率是骨关节炎等人群的近2.5倍。其根本原因是OP患者“成骨-破骨微环境失衡”的病理效应。当假体植入OP患者体内后,在假体移植区域的骨形成作用明显低于骨吸收,钙磷代谢不平衡导致关节严重的骨质流失,脆弱的骨质条件无法产生长期支撑假体的力学负荷,从而导致假体松动和假体周围骨折等严重术后并发症。因此,如何纠正OP患者“成骨-破骨微环境”的代谢失衡状态,以降低OP患者关节置换术后的并发症发生率,这一科学问题亟需解决。
目前,临床上广泛使用的多孔钛合金植入物并未具备调节成骨-破骨微环境失衡的功能。此外,钛合金材料具有较高的生物惰性和表面光滑特性,限制了其在微孔内促进成骨作用的效率。同时,由于多孔钛合金具有开放的多孔结构,常规的改性方法难以在其表面实现均匀分布的涂层。为了克服现有多孔钛合金的上述限制,开展在其表面制备具有调节骨质疏松患者“成骨-破骨微环境”代谢失衡状态的生物活性涂层的研究,成为解决上述问题的有效途径。
双磷酸盐作为临床一线抗骨质疏松药物,能够通过多种途径发挥其效应。它具有抑制破骨前体细胞的破骨分化、抑制破骨细胞的增殖、促进破骨细胞凋亡的能力,并且能够调节成骨细胞及骨髓间充质干细胞的成骨能力,因此具备逆转破骨-成骨微环境失衡的功能。然而,双磷酸盐在口服和静脉注射等系统性用药方式下的生物利用率较低,导致其到达假体与宿主骨整合界面的药物浓度不足,难以有效地发挥调节作用。这种情况使得精准调控假体界面的“成骨-破骨平衡”成为一项挑战。
中空介孔二氧化硅纳米颗粒(hollow mesoporous silica nanoparticles,HMSNs)是一种特殊类型的基于二氧化硅合成的纳米材料,内部具有较大的空腔,其外壳上具有通透的介孔通道。HMSN 具有独特的结构特征:首先,HMSNs 的中空内部可用于负载药物。其次,带有介孔结构的二氧化硅外壳使得药物能够通过壳进行自由扩散。其具有以下特征:1. 可调且狭窄的孔径分布(2-30nm);2. 可调式多孔结构;3. 较高的比表面积(最高可达 1500 cm2/g);4. 高容积(约1 cm3/g)。因为 HMSNs的这些特性,其已经被广泛用于生物医药领域。目前,还没有构建HMSNs涂层于多孔钛合金植入物表面并负载双磷酸盐,以构建生物活性界面的报道。
发明内容
本发明的目的在于提供一种在多孔钛合金植入物表面制备中空介孔二氧化硅纳米颗粒涂层,并通过负载双磷酸盐实现在钛合金植入物构建生物活性界面的功能。
一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的制备方法,经过合成中空介孔二氧化硅纳米颗粒(HMSNs,Hollow Mesoporous Silica Nanoparticles),并将其涂覆于多孔钛合金植入物表面,形成一种纳米结构涂层;
具体包括如下步骤:
(1)HMSNs的制备:将1-5ml氨水、10-80ml无水乙醇和1-10ml去离子水共混,25-60℃温度下搅拌1-6h,得到混合溶液①,将所得混合溶液①放入离心机离心(5min)、在(60)温度下干燥(0.5)h,得到固体二氧化硅粉末;将0.1-1.0g CTAB、20-200ml无水乙醇、20-200ml去离子水和1-5ml氨水混合制得混合溶液②,取制得的二氧化硅粉末0.2-0.8g置入上述混合溶液②中超声震荡1-6h,再加入0.5-5ml TEOS溶液,超声震荡4-8h得到混合溶液③;将混合溶液③放入离心机离心5min,并用去离子水洗涤3次,-40℃冷冻干燥,获得白色粉末;取上述所得白色粉末0.1g-1g加入至0.2M-0.8M的碳酸钠溶液中,在45-90℃温度下搅拌1-6h,离心5min并用去离子水洗涤3次,获得含有CTAB二氧化硅外壳的纳米颗粒;将含有CTAB二氧化硅外壳的纳米颗粒置于500-600℃马弗炉中煅烧2-8h,去除CTAB,获得中空介孔二氧化硅纳米颗粒(HMSNs);
(2)多孔钛合金植入物的表面预处理:将多孔钛合金植入物,依次置于丙酮、去离子水和无水乙醇中,进行超声清洗,每个环节超声清洗的时间为10-20min,将超声清洗完成后的多孔钛合金植入物置于100℃烘箱干燥10min-60min;然后将多孔钛合金植入物置于piranha溶液中(浓硫酸:30%双氧水=3:1)浸泡5-20min,取出后使用去离子水冲洗,用氮气吹干;
(3)多孔钛合金植入物表面聚合物粘结层的制备:多孔钛合金植入物表面聚合物粘结层的制备:将经过步骤(2)处理的多孔钛合金植入物浸入0.05-0.5wt%的聚二烯丙基二甲基氯化铵(Poly dimethyl diallyl ammonium chloride,PDDA)溶液中,浸入时间为5-10min,取出后用去离子水清洗,氮气烘干;再将多孔钛合金植入物浸入0.05-0.5wt%的聚丙烯酸(Polyacrylic acid,PAA)溶液中,浸入时间为5-10min,取出后用去离子水清洗,氮气烘干;重复上述两个过程2-4次;
(4)HMSNs涂层制备:将经过步骤(3)处理的多孔钛合金植入物浸入0.05-0.5wt%PDDA溶液中,浸入时间为5-10min;取出后用去离子水清洗,氮气烘干;再将多孔钛合金植入物浸入到步骤(1)得到的0.05-0.5wt%HMSN溶液中,浸入时间为5-10min,取出后用去离子水清洗,氮气烘干;重复上述两个过程1-6次;
(5)将步骤(4)制备的多孔钛合金植入物在400-600℃条件下煅烧2-6h,升温速率为1-3℃/min,去除涂层中的有机物,从而在多孔钛合金表面构建了HMSNs涂层。
所述的多孔钛合金植入物孔径为400-800μm,孔隙率为50-80%。
所述的HMSNs结构中,介孔孔径为2.0-3.9nm。
所述的步骤(4)中HMSNs的重量百分比为0.3-0.5wt%。
所述的步骤(5)中煅烧温度为500-550℃,煅烧时间为2-4h。
一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的应用,将构建了HMSNs涂层的多孔钛合金植入物置于双磷酸盐溶液中,在室温条件下振荡12-48h,完成双磷酸盐的负载。
所述的双磷酸盐溶液为20μg-2mg/ml的唑来膦酸溶液。
本发明的有益效果:
1.中空介孔二氧化硅纳米颗粒具有较高生物相容性,且其中空空腔结构和有序的介孔结构,具有较高的载药能力。
2.HMSNs能够均匀分布在多孔钛合金植入物表面及内部小梁结构,有利于细胞附着,提高了多孔钛合金植入物的生物活性。
3.本发明中HMSNs涂层制备不受基体形状限制,可以在形状复杂的基体上均匀的制备生物活性涂层。
4.本发明HMSNs涂层能够吸附并缓释双磷酸盐,具有调控植入物周围微环境成骨-破骨平衡的生物功能。
附图说明
图1:为本发明实施例1多孔钛合金植入物表面HMSNs涂层的SEM图片。
图2:为本发明实施例1多孔钛合金植入物表面HMSNs涂层的截面SEM图片。
图3:为本发明实施例1多孔钛合金植入物表面HMSNs涂层的XRD图片。
图4:为本发明实施例2多孔钛合金植入物表面生物活性HMSNs涂层的TEM-EDS。
图5:为本发明实施例3的各组TRAP染色结果。
图6:为本发明实施例3的各组ALP染色。
图7:为本发明对比例1多孔钛合金表面HMSNs涂层的SEM图片。
图8:为本发明对比例1多孔钛合金表面HMSNs涂层的截面SEM图片。
图1所示:本发明实施例1HMSNs在多孔钛合金基底表面均匀涂覆,表现较强的成膜性,且纳米颗粒之间交错排列,形成凹凸不平的界面,增加了基底的粗糙度,有利于细胞的粘附。
图2所示:本发明实施例1 HMSNs涂层厚度约为8μm。
图3所示:本发明实施例1HMSNs存在典型的衍射峰,说明涂层过程未对纳米颗粒结构产生不利影响。
图4所示:本发明实施例2说明HMSNs涂层成功负载唑来膦酸。
图5和6所示:本发明实施例3的生物活性HMSNs涂层能够抑制破骨细胞的形成(Trap染色提示破骨细胞数量减少),同时能够促进骨髓间充质干细胞碱性磷酸酶的表达(ALP染色颜色明显加深),发挥调控微环境成骨-破骨平衡的生物功能。
图8所示:本发明对比例1改变HMSNs涂覆次数后的多孔钛合金表面形貌,与实施例1对比发现,仅涂覆2次时HMSNs涂层分布显著不均匀。
具体实施方式:
本发明涉及到的实施例所用多孔钛合金具有开放多孔状结构,其结构参数如下:本发明多孔钛合金采用的是Ti6Al4V,具有开放多孔状结构,孔径为400-800μm,孔隙率为50-80%。所述的HMSNs结构中,介孔孔径为2.0-3.9nm。
实施例
请参阅图1、图2和图3。
一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的制备方法,经过合成中空介孔二氧化硅纳米颗粒(HMSNs,Hollow Mesoporous Silica Nanoparticles),并将其涂覆于多孔钛合金植入物表面,形成一种纳米结构涂层;
具体包括如下步骤:
(1)HMSNs的制备:将3ml氨水、65ml无水乙醇和10ml去离子水共混,25℃温度下搅拌3h,得到混合溶液①,将所得混合溶液①放入离心机离心5min、在60℃温度下干燥0.5h,得到固体二氧化硅粉末;将0.8g CTAB、160ml无水乙醇、160ml去离子水和3ml氨水混合制得混合溶液②,取制得的二氧化硅粉末0.6g置入上述混合溶液②中超声震荡2h,再加入4mlTEOS溶液,超声震荡6h得到混合溶液③;将混合溶液③放入离心机离心5min,并用去离子水洗涤3次,在-40℃条件下冷冻干燥,获得白色粉末;取上述所得白色粉末0.5g加入至0.8M的碳酸钠溶液中,在80℃温度下搅拌6h,离心5min并用去离子水洗涤3次,获得含有CTAB二氧化硅外壳的纳米颗粒;将含有CTAB二氧化硅外壳的纳米颗粒置于550℃马弗炉中煅烧8h,去除CTAB,获得中空介孔二氧化硅纳米颗粒(HMSNs);
(2)多孔钛合金植入物的表面预处理:将多孔钛合金植入物,依次置于丙酮、去离子水和无水乙醇中,进行超声清洗,每个环节超声清洗的时间为20min,将超声清洗完成后的多孔钛合金植入物置于100℃烘箱干燥30min;然后将多孔钛合金植入物置于piranha溶液中(浓硫酸:30%双氧水=3:1)浸泡10min,取出后使用去离子水冲洗,用氮气吹干;
(3)多孔钛合金植入物表面聚合物粘结层的制备:多孔钛合金植入物表面聚合物粘结层的制备:将经过步骤(2)处理的多孔钛合金植入物浸入0.5wt%的聚二烯丙基二甲基氯化铵(Poly dimethyl diallyl ammonium chloride,PDDA)溶液中,浸入时间为5min,取出后用去离子水清洗,氮气烘干;再将多孔钛合金植入物浸入0.5wt%的聚丙烯酸(Polyacrylic acid,PAA)溶液中,浸入时间为5min,取出后用去离子水清洗,氮气烘干;重复上述两个过程3次;
(4)HMSNs涂层制备:将经过步骤(3)处理的多孔钛合金植入物浸入0.5wt% PDDA溶液中,浸入时间为5min;取出后用去离子水清洗,氮气烘干;再将多孔钛合金植入物浸入到步骤(1)得到的0.5wt%HMSN溶液中,浸入时间为5min,取出后用去离子水清洗,氮气烘干;重复上述两个过程6次;
(5)将步骤(4)制备的多孔钛合金植入物在550℃条件下煅烧4h,升温速率为2℃/min,去除涂层中的有机物,从而在多孔钛合金表面构建了HMSNs涂层。
实施例2
请参阅图4。
一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的应用,经过合成中空介孔二氧化硅纳米颗粒(HMSNs,Hollow Mesoporous Silica Nanoparticles),并将其涂覆于多孔钛合金植入物表面,形成一种纳米结构涂层;将构建了HMSNs涂层的多孔钛合金植入物置于双磷酸盐溶液中,完成双磷酸盐的负载。
具体包括如下步骤:
(1)HMSNs的制备:将3ml氨水、20ml无水乙醇和10ml去离子水共混,37℃温度下搅拌1h,得到混合溶液①,将所得混合溶液①放入离心机离心5min、在60℃温度下干燥0.5h,得到固体二氧化硅粉末;将0.5g CTAB、100ml无水乙醇、100ml去离子水和2ml氨水混合制得混合溶液②,取制得的二氧化硅粉末0.5g置入上述混合溶液②中超声震荡1h,再加入1.5mlTEOS溶液,超声震荡8h得到混合溶液③;将混合溶液③放入离心机离心5min,并用去离子水洗涤3次,在-40℃条件下冷冻干燥,获得白色粉末;取上述所得白色粉末0.5g加入至0.8M的碳酸钠溶液中,在80℃温度下搅拌5h,离心5min并用去离子水洗涤3次,获得含有CTAB二氧化硅外壳的纳米颗粒;将含有CTAB二氧化硅外壳的纳米颗粒置于600℃马弗炉中煅烧6h,去除CTAB,获得中空介孔二氧化硅纳米颗粒(HMSNs);
(2)多孔钛合金植入物的表面预处理:将多孔钛合金植入物,依次置于丙酮、去离子水和无水乙醇中,进行超声清洗,每个环节超声清洗的时间为15min,将超声清洗完成后的多孔钛合金植入物置于100℃烘箱干燥30min;然后将多孔钛合金植入物置于piranha溶液中(浓硫酸:30%双氧水=3:1)浸泡10min,取出后使用去离子水冲洗,用氮气吹干;
(3)多孔钛合金植入物表面聚合物粘结层的制备:多孔钛合金植入物表面聚合物粘结层的制备:将经过步骤(2)处理的多孔钛合金植入物浸入0.3wt%的聚二烯丙基二甲基氯化铵(Poly dimethyl diallyl ammonium chloride,PDDA)溶液中,浸入时间为5min,取出后用去离子水清洗,氮气烘干;再将多孔钛合金植入物浸入0.3wt%的聚丙烯酸(Polyacrylic acid,PAA)溶液中,浸入时间为5min,取出后用去离子水清洗,氮气烘干;重复上述两个过程3次;
(4)HMSNs涂层制备:将经过步骤(3)处理的多孔钛合金植入物浸入0.3wt% PDDA溶液中,浸入时间为10min;取出后用去离子水清洗,氮气烘干;再将多孔钛合金植入物浸入到步骤(1)得到的0.3wt%HMSN溶液中,浸入时间为10min,取出后用去离子水清洗,氮气烘干;重复上述两个过程4次;
(5)将步骤(4)制备的多孔钛合金植入物在500℃条件下煅烧6h,升温速率为2℃/min,去除涂层中的有机物,从而在多孔钛合金表面构建了HMSNs涂层。
将HMSNs涂层的多孔钛合金置于40μg/ml唑来膦酸溶液中,在室温条件下振荡24h,通过纳米颗粒有序的介孔孔径和中空空腔结构吸附唑来膦酸,完成多孔钛合金表面生物活性涂层的构建。
实施例3
请参阅图5、图6。
通过实施例3验证多孔钛合金植入物表面构建HMSNs的生物活性涂层调控成骨-破骨平衡的能力。
调控破骨过程相关实验如下:
在6孔板中,每孔将2×104个破骨前体细胞RAW264 .7与生物活性涂层的多孔钛合金共培养,其中加入含有破骨诱导因子RANKL(100ng/ml)的MEM-α培养基,诱导RANW264 .7细胞定向分化为破骨细胞,培养4天后使用抗酒石酸酸性磷酸酶(TRAP)染色试剂盒,对破骨细胞形成的数量进行统计。
调控成骨过程相关实验如下:
在24孔板中,每孔将2×104个BMSCs与生物活性涂层的多孔钛合金共培养,使用成骨诱导培养基(主要成分为10%胎牛血清,1%青链霉素双抗,12.8mg/L维生素C,2 .16g/Lβ-甘油磷酸钠,5mmol/L地塞米松)进行成骨诱导培养,培养14天后使用碱性磷酸酶(ALP)染色试剂盒,进行ALP的定量及定性分析。
实施例4
一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的制备方法,经过合成中空介孔二氧化硅纳米颗粒(HMSNs,Hollow Mesoporous Silica Nanoparticles),并将其涂覆于多孔钛合金植入物表面,形成一种纳米结构涂层;
具体包括如下步骤:
(1)HMSNs的制备:将3ml氨水、20ml无水乙醇和10ml去离子水共混,37℃温度下搅拌1h,得到混合溶液①,将所得混合溶液①放入离心机离心5min、在60℃温度下干燥0.5h,得到固体二氧化硅粉末;将0.5g CTAB、100ml无水乙醇、100ml去离子水和2ml氨水混合制得混合溶液②,取制得的二氧化硅粉末0.5g置入上述混合溶液②中超声震荡1h,再加入1.5mlTEOS溶液,超声震荡8h得到混合溶液③;将混合溶液③放入离心机离心5min,并用去离子水洗涤3次,在-40℃条件下冷冻干燥,获得白色粉末;取上述所得白色粉末0.5g加入至0.8M的碳酸钠溶液中,在80℃温度下搅拌5h,离心5min并用去离子水洗涤3次,获得含有CTAB二氧化硅外壳的纳米颗粒;将含有CTAB二氧化硅外壳的纳米颗粒置于600℃马弗炉中煅烧6h,去除CTAB,获得中空介孔二氧化硅纳米颗粒(HMSNs);
(2)多孔钛合金植入物的表面预处理:将多孔钛合金植入物,依次置于丙酮、去离子水和无水乙醇中,进行超声清洗,每个环节超声清洗的时间为20min,将超声清洗完成后的多孔钛合金植入物置于100℃烘箱干燥30min;然后将多孔钛合金植入物置于piranha溶液中(浓硫酸:30%双氧水=3:1)浸泡10min,取出后使用去离子水冲洗,用氮气吹干;
(3)多孔钛合金植入物表面聚合物粘结层的制备:多孔钛合金植入物表面聚合物粘结层的制备:将经过步骤(2)处理的多孔钛合金植入物浸入0.5wt%的聚二烯丙基二甲基氯化铵(Poly dimethyl diallyl ammonium chloride,PDDA)溶液中,浸入时间为5min,取出后用去离子水清洗,氮气烘干;再将多孔钛合金植入物浸入0.5wt%的聚丙烯酸(Polyacrylic acid,PAA)溶液中,浸入时间为5min,取出后用去离子水清洗,氮气烘干;重复上述两个过程3次;
(4)HMSNs涂层制备:将经过步骤(3)处理的多孔钛合金植入物浸入0.5wt% PDDA溶液中,浸入时间为5min;取出后用去离子水清洗,氮气烘干;再将多孔钛合金植入物浸入到步骤(1)得到的0.5wt%HMSN溶液中,浸入时间为5min,取出后用去离子水清洗,氮气烘干;重复上述两个过程2次;
(5)将步骤(4)制备的多孔钛合金植入物在550℃条件下煅烧4h,升温速率为2℃/min,去除涂层中的有机物,从而在多孔钛合金表面构建了HMSNs涂层。
将实施例1和实施例4进行对比,二者在步骤(4)中的重复浸泡于HMSNs溶液中的次数不同,观察实施例4改变HMSNs涂覆次数后的多孔钛合金植入物表面形貌,较涂覆2次时分子筛涂层分布显著不均匀。通过对比,可以得出结论:HMSNs涂覆次数对涂层形貌具有较大影响。
Claims (7)
1. 一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的制备方法,其特征在于:经过合成中空介孔二氧化硅纳米颗粒(HMSNs,Hollow Mesoporous Silica Nanoparticles),并将其涂覆于多孔钛合金植入物表面,形成一种纳米结构涂层;
具体包括如下步骤:
(1)HMSNs的制备:将1-5ml氨水、10-80ml无水乙醇和1-10ml去离子水共混,25-60℃温度下搅拌1-6h,得到混合溶液①,将所得混合溶液①放入离心机离心5min、在60℃温度下干燥0.5h,得到固体二氧化硅粉末;将0.1-1.0g CTAB、20-200ml无水乙醇、20-200ml去离子水和1-5ml氨水混合制得混合溶液②,取制得的二氧化硅粉末0.2-0.8g置入上述混合溶液②中超声震荡1-6h,再加入0.5-5ml TEOS溶液,超声震荡4-8h得到混合溶液③;将混合溶液③放入离心机离心5min,并用去离子水洗涤3次,在-40℃条件下冷冻干燥,获得白色粉末;取上述所得白色粉末0.1g-1g加入至0.2M-0.8M的碳酸钠溶液中,在45-90℃温度下搅拌1-6h,离心5min并用去离子水洗涤3次,获得含有CTAB二氧化硅外壳的纳米颗粒;将含有CTAB二氧化硅外壳的纳米颗粒置于500-600℃马弗炉中煅烧2-8h,去除CTAB,获得中空介孔二氧化硅纳米颗粒(HMSNs);
(2)多孔钛合金植入物的表面预处理:将多孔钛合金植入物,依次置于丙酮、去离子水和无水乙醇中,进行超声清洗,每个环节超声清洗的时间为10-20min,将超声清洗完成后的多孔钛合金植入物置于100℃烘箱干燥10min-60min;然后将多孔钛合金植入物置于piranha溶液中(浓硫酸:30%双氧水=3:1)浸泡5-20min,取出后使用去离子水冲洗,用氮气吹干;
(3)多孔钛合金植入物表面聚合物粘结层的制备:多孔钛合金植入物表面聚合物粘结层的制备:将经过步骤(2)处理的多孔钛合金植入物浸入0.05-0.5wt%的聚二烯丙基二甲基氯化铵(Poly dimethyl diallyl ammonium chloride,PDDA)溶液中,浸入时间为5-10min,取出后用去离子水清洗,氮气烘干;再将多孔钛合金植入物浸入0.05-0.5wt%的聚丙烯酸(Polyacrylic acid,PAA)溶液中,浸入时间为5-10min,取出后用去离子水清洗,氮气烘干;重复上述两个过程2-4次;
(4)HMSNs涂层制备:将经过步骤(3)处理的多孔钛合金植入物浸入0.05-0.5wt% PDDA溶液中,浸入时间为5-10min;取出后用去离子水清洗,氮气烘干;再将多孔钛合金植入物浸入到步骤(1)得到的0.05-0.5wt%HMSN溶液中,浸入时间为5-10min,取出后用去离子水清洗,氮气烘干;重复上述两个过程1-6次;
(5)将步骤(4)制备的多孔钛合金植入物在400-600℃条件下煅烧2-6h,升温速率为1-3℃/min,去除涂层中的有机物,从而在多孔钛合金表面构建了HMSNs涂层。
2.根据权利要求1所述的一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的制备方法,其特征在于:所述的多孔钛合金植入物孔径为400-800μm,孔隙率为50-80%。
3.根据权利要求1所述的一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的制备方法,其特征在于:所述的HMSNs结构中,介孔孔径为2.0-3.9nm。
4.根据权利要求1所述的一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的制备方法,其特征在于:所述的步骤(4)中HMSNs的重量百分比为0.3-0.5wt%。
5.根据权利要求1所述的一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的制备方法,其特征在于:所述的步骤(5)中煅烧温度为500-550℃,煅烧时间为2-4h。
6.一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的应用,其特征在于:将构建了HMSNs涂层的多孔钛合金植入物置于双磷酸盐溶液中,在室温条件下振荡12-48h,完成双磷酸盐的负载。
7.根据权利要求6所述的一种多孔钛合金表面中空介孔二氧化硅纳米颗粒涂层的应用,其特征在于:所述的双磷酸盐溶液为20μg-2mg/ml的唑来膦酸溶液。
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