CN113069597A - 一种溶胶-凝胶法制备掺杂二氧化钛陶瓷薄膜的方法 - Google Patents
一种溶胶-凝胶法制备掺杂二氧化钛陶瓷薄膜的方法 Download PDFInfo
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Abstract
一种溶胶‑凝胶法制备掺杂二氧化钛陶瓷薄膜的方法,在传统的覆有二氧化钛陶瓷薄膜的血管支架的基础上,通过溶胶‑凝胶法向薄膜中掺入了石墨烯材料,对二氧化钛陶瓷薄膜的血液相容性进行了改良。进一步地,本发明研究了不同石墨烯掺杂量对血液相容性的影响,研究表明在掺入量为5%‑10.8%时,能够使得血管支架表面二氧化钛陶瓷薄膜的溶血率低于10%,在掺入量为7.3%时,更能使溶血率低至2.1%。
Description
技术领域
本发明涉及陶瓷材料领域,具体涉及一种溶胶-凝胶法制备掺杂二氧化钛陶瓷薄膜的方法。
背景技术
血管支架是临床医疗中广泛应用的医用材料,其植入病变血管,经历压卧、植入、球囊扩张、回弹等过程,引起血管内血流动力学变化以及支架段血管组织的力学微环境变化。理想的血管支架再植入体内6个月后病变部位不会在发生再狭窄。
对于不同类型的血管支架,基体材料的要求可能不同,如对于聚合物支架,强度和尺寸稳定性是其首要考虑的,而抗腐蚀性能、拉伸强度则是金属支架最重要的化学特性。金属支架是临床应用比较广泛的支架种类,常见的主要有镁合金、316L不锈钢、钛合金、钴铬合金和镍钛记忆合金支架等。为了提高金属支架的耐腐蚀性能,现有技术中常采用的方式是在支架表面涂覆镀层,与此同时,镀层支架材料的血液相容性是医疗实践中必须考量的重要因素。因此,如何提高镀层支架材料的血液相容性是一项值得长期探究的课题。
发明内容
针对现有技术存在的问题,本发明旨在提供一种掺杂二氧化钛陶瓷薄膜的方法,该方法通过溶胶-凝胶法向血管支架表面二氧化钛陶瓷薄膜掺入石墨烯,得到了血液相容性优异的石墨烯掺杂二氧化钛陶瓷薄膜。
一种溶胶-凝胶法制备掺杂二氧化钛陶瓷薄膜的方法,包括以下步骤:
A.以血管支架材料为衬底;
B.对衬底进行预处理,预处理包括脱脂、打磨、清洗和烘干,其中脱脂选用碳酸钠溶液,清洗选用无水乙醇并配合超声波辅助;
C.制备MgO过渡层:将烘干的医用镁合金放入溅射镀膜设备中,以MgO靶为溅射源,在氩气气氛下制备MgO过渡层,其中电源功率为60-80W,氩气流量60-90sccm,衬底温度150-180℃,溅射时间18-30min;
D.将钛酸丁酯和无水乙醇混合得到溶液A,以无水乙醇和蒸馏水混合并添加石墨烯得到石墨烯分散液,用冰醋酸调节pH值后得到溶液B,将溶液A滴加到溶液B中,滴加过程中不断搅拌,陈化后得到溶胶,其中钛酸丁酯的用量为5-8mol,无水乙醇的用量为40-50mol,蒸馏水的用量为4-10mol,冰醋酸的用量为3.5-5mol,陈化时间为12-24h;
E.通过提拉法制备石墨烯掺杂二氧化钛陶瓷薄膜,以5-8cm/min提拉速度涂覆上述溶胶,而后分别在80-90℃下干燥20-25min,在45-50℃下干燥20-30min,在25-30℃下干燥30-50min,自然冷却到室温,在300-350℃下烧结30-40min,烧结后根据薄膜厚度多次涂膜,最后在450-500℃下退火1-2h,得到厚度为3-5μm的石墨烯掺杂二氧化钛陶瓷薄膜。
进一步地,所述衬底为10×10*1.5mm的基片。
进一步地,所述碱性溶液的浓度为20-30wt%。
进一步地,所述衬底为医用镁合金、316L不锈钢、钛合金、钴铬合金或镍钛记忆合金。
进一步地,所述石墨烯的用量为整个溶胶质量的5%-10.8%。
进一步地,所述石墨烯的用量为整个溶胶的质量7.3%。。
进一步地,所述碳酸钠溶液的浓度为20%-30%。
本发明在传统的覆有二氧化钛陶瓷薄膜的血管支架的基础上,通过溶胶-凝胶法向薄膜中掺入了石墨烯材料,对二氧化钛陶瓷薄膜的血液相容性进行了改良。进一步地,本发明研究了不同石墨烯掺杂量对血液相容性的影响,研究表明在掺入量为5%-10.8%时,能够使得血管支架表面二氧化钛陶瓷薄膜的溶血率低于10%,在掺入量为7.3%时,更能使溶血率低至2.1%。
具体实施方式
下面通过具体实施例来验证本发明的技术效果,但是本发明的实施方式不局限于此。
实施例1
一种溶胶-凝胶法制备掺杂二氧化钛陶瓷薄膜的方法,包括以下步骤:
A.以医用镁合金为衬底材料,将医用镁合金切割成10×10*1.5mm的基片;
B.对衬底进行预处理,预处理包括脱脂、打磨、清洗和烘干,其中脱脂选用浓度为20%的碳酸钠溶液,清洗选用无水乙醇并配合超声波辅助;
C.制备MgO过渡层:将烘干的医用镁合金放入溅射镀膜设备中,以MgO靶为溅射源,在氩气气氛下制备MgO过渡层,其中电源功率为60W,氩气流量60sccm,衬底温度150℃,溅射时间18min;
D.将钛酸丁酯和无水乙醇混合得到溶液A,以无水乙醇和蒸馏水混合并添加石墨烯得到石墨烯分散液,用冰醋酸调节pH值后得到溶液B,将溶液A滴加到溶液B中,滴加过程中不断搅拌,陈化后得到溶胶,其中钛酸丁酯的用量为5mol,无水乙醇的用量为40mol,蒸馏水的用量为4mol,冰醋酸的用量为3.5mol,石墨烯的用量为整个溶胶的5wt.%,陈化时间为12h;
E.通过提拉法制备石墨烯掺杂二氧化钛陶瓷薄膜,以5cm/min提拉速度涂覆上述溶胶,而后分别在80℃下干燥20min,在45℃下干燥20min,在25℃下干燥30min,自然冷却到室温,在300℃下烧结30min,烧结后根据薄膜厚度多次涂膜,最后在450℃下退火1h,得到厚度为3μm的石墨烯掺杂二氧化钛陶瓷薄膜。
实施例2
一种溶胶-凝胶法制备掺杂二氧化钛陶瓷薄膜的方法,包括以下步骤:
A.以医用镁合金为衬底材料,将医用镁合金切割成10×10*1.5mm的基片;
B.对衬底进行预处理,预处理包括脱脂、打磨、清洗和烘干,其中脱脂选用浓度为20%的碳酸钠溶液,清洗选用无水乙醇并配合超声波辅助;
C.制备MgO过渡层:将烘干的医用镁合金放入溅射镀膜设备中,以MgO靶为溅射源,在氩气气氛下制备MgO过渡层,其中电源功率为60W,氩气流量60sccm,衬底温度150℃,溅射时间18min;
D.将钛酸丁酯和无水乙醇混合得到溶液A,以无水乙醇和蒸馏水混合并添加石墨烯得到石墨烯分散液,用冰醋酸调节pH值后得到溶液B,将溶液A滴加到溶液B中,滴加过程中不断搅拌,陈化后得到溶胶,其中钛酸丁酯的用量为5mol,无水乙醇的用量为40mol,蒸馏水的用量为4mol,冰醋酸的用量为3.5mol,石墨烯的用量为整个溶胶的7.3wt.%,陈化时间为12h;
E.通过提拉法制备石墨烯掺杂二氧化钛陶瓷薄膜,以5cm/min提拉速度涂覆上述溶胶,而后分别在80℃下干燥20min,在45℃下干燥20min,在25℃下干燥30min,自然冷却到室温,在300℃下烧结30min,烧结后根据薄膜厚度多次涂膜,最后在450℃下退火1h,得到厚度为3μm的石墨烯掺杂二氧化钛陶瓷薄膜。
实施例3
一种溶胶-凝胶法制备掺杂二氧化钛陶瓷薄膜的方法,包括以下步骤:
A.以医用镁合金为衬底材料,将医用镁合金切割成10×10*1.5mm的基片;
B.对衬底进行预处理,预处理包括脱脂、打磨、清洗和烘干,其中脱脂选用浓度为20%的碳酸钠溶液,清洗选用无水乙醇并配合超声波辅助;
C.制备MgO过渡层:将烘干的医用镁合金放入溅射镀膜设备中,以MgO靶为溅射源,在氩气气氛下制备MgO过渡层,其中电源功率为60W,氩气流量60sccm,衬底温度150℃,溅射时间18min;
D.将钛酸丁酯和无水乙醇混合得到溶液A,以无水乙醇和蒸馏水混合并添加石墨烯得到石墨烯分散液,用冰醋酸调节pH值后得到溶液B,将溶液A滴加到溶液B中,滴加过程中不断搅拌,陈化后得到溶胶,其中钛酸丁酯的用量为5mol,无水乙醇的用量为40mol,蒸馏水的用量为4mol,冰醋酸的用量为3.5mol,石墨烯的用量为整个溶胶的9.5wt.%,陈化时间为12h;
E.通过提拉法制备石墨烯掺杂二氧化钛陶瓷薄膜,以5cm/min提拉速度涂覆上述溶胶,而后分别在80℃下干燥20min,在45℃下干燥20min,在25℃下干燥30min,自然冷却到室温,在300℃下烧结30min,烧结后根据薄膜厚度多次涂膜,最后在450℃下退火1h,得到厚度为3μm的石墨烯掺杂二氧化钛陶瓷薄膜。
实施例4
一种溶胶-凝胶法制备掺杂二氧化钛陶瓷薄膜的方法,包括以下步骤:
A.以医用镁合金为衬底材料,将医用镁合金切割成10×10*1.5mm的基片;
B.对衬底进行预处理,预处理包括脱脂、打磨、清洗和烘干,其中脱脂选用浓度为20%的碳酸钠溶液,清洗选用无水乙醇并配合超声波辅助;
C.制备MgO过渡层:将烘干的医用镁合金放入溅射镀膜设备中,以MgO靶为溅射源,在氩气气氛下制备MgO过渡层,其中电源功率为60W,氩气流量60sccm,衬底温度150℃,溅射时间18min;
D.将钛酸丁酯和无水乙醇混合得到溶液A,以无水乙醇和蒸馏水混合并添加石墨烯得到石墨烯分散液,用冰醋酸调节pH值后得到溶液B,将溶液A滴加到溶液B中,滴加过程中不断搅拌,陈化后得到溶胶,其中钛酸丁酯的用量为5mol,无水乙醇的用量为40mol,蒸馏水的用量为4mol,冰醋酸的用量为3.5mol,石墨烯的用量为整个溶胶的10.8wt.%,陈化时间为12h;
E.通过提拉法制备石墨烯掺杂二氧化钛陶瓷薄膜,以5cm/min提拉速度涂覆上述溶胶,而后分别在80℃下干燥20min,在45℃下干燥20min,在25℃下干燥30min,自然冷却到室温,在300℃下烧结30min,烧结后根据薄膜厚度多次涂膜,最后在450℃下退火1h,得到厚度为3μm的石墨烯掺杂二氧化钛陶瓷薄膜。
对比例1
一种溶胶-凝胶法制备掺杂二氧化钛陶瓷薄膜的方法,包括以下步骤:
A.以医用镁合金为衬底材料,将医用镁合金切割成10×10*1.5mm的基片;
B.对衬底进行预处理,预处理包括脱脂、打磨、清洗和烘干,其中脱脂选用浓度为20%的碳酸钠溶液,清洗选用无水乙醇并配合超声波辅助;
C.制备MgO过渡层:将烘干的医用镁合金放入溅射镀膜设备中,以MgO靶为溅射源,在氩气气氛下制备MgO过渡层,其中电源功率为60W,氩气流量60sccm,衬底温度150℃,溅射时间18min;
D.将钛酸丁酯和无水乙醇混合得到溶液A,以无水乙醇和蒸馏水混合并添加石墨烯得到石墨烯分散液,用冰醋酸调节pH值后得到溶液B,将溶液A滴加到溶液B中,滴加过程中不断搅拌,陈化后得到溶胶,其中钛酸丁酯的用量为5mol,无水乙醇的用量为40mol,蒸馏水的用量为4mol,冰醋酸的用量为3.5mol,石墨烯的用量为整个溶胶的3.0wt.%,陈化时间为12h;
E.通过提拉法制备石墨烯掺杂二氧化钛陶瓷薄膜,以5cm/min提拉速度涂覆上述溶胶,而后分别在80℃下干燥20min,在45℃下干燥20min,在25℃下干燥30min,自然冷却到室温,在300℃下烧结30min,烧结后根据薄膜厚度多次涂膜,最后在450℃下退火1h,得到厚度为3μm的石墨烯掺杂二氧化钛陶瓷薄膜。
对比例2
一种溶胶-凝胶法制备掺杂二氧化钛陶瓷薄膜的方法,包括以下步骤:
A.以医用镁合金为衬底材料,将医用镁合金切割成10×10*1.5mm的基片;
B.对衬底进行预处理,预处理包括脱脂、打磨、清洗和烘干,其中脱脂选用浓度为20%的碳酸钠溶液,清洗选用无水乙醇并配合超声波辅助;
C.制备MgO过渡层:将烘干的医用镁合金放入溅射镀膜设备中,以MgO靶为溅射源,在氩气气氛下制备MgO过渡层,其中电源功率为60W,氩气流量60sccm,衬底温度150℃,溅射时间18min;
D.将钛酸丁酯和无水乙醇混合得到溶液A,以无水乙醇和蒸馏水混合并添加石墨烯得到石墨烯分散液,用冰醋酸调节pH值后得到溶液B,将溶液A滴加到溶液B中,滴加过程中不断搅拌,陈化后得到溶胶,其中钛酸丁酯的用量为5mol,无水乙醇的用量为40mol,蒸馏水的用量为4mol,冰醋酸的用量为3.5mol,石墨烯的用量为整个溶胶的12.5wt.%,陈化时间为12h;
E.通过提拉法制备石墨烯掺杂二氧化钛陶瓷薄膜,以5cm/min提拉速度涂覆上述溶胶,而后分别在80℃下干燥20min,在45℃下干燥20min,在25℃下干燥30min,自然冷却到室温,在300℃下烧结30min,烧结后根据薄膜厚度多次涂膜,最后在450℃下退火1h,得到厚度为3μm的石墨烯掺杂二氧化钛陶瓷薄膜。
对比例3
一种溶胶-凝胶法制备二氧化钛陶瓷薄膜的方法,包括以下步骤:
A.以医用镁合金为衬底材料,将医用镁合金切割成10×10*1.5mm的基片;
B.对衬底进行预处理,预处理包括脱脂、打磨、清洗和烘干,其中脱脂选用浓度为20%的碳酸钠溶液,清洗选用无水乙醇并配合超声波辅助;
C.制备MgO过渡层:将烘干的医用镁合金放入溅射镀膜设备中,以MgO靶为溅射源,在氩气气氛下制备MgO过渡层,其中电源功率为60W,氩气流量60sccm,衬底温度150℃,溅射时间18min;
D.将钛酸丁酯和无水乙醇混合得到溶液A,以无水乙醇和蒸馏水混合并用冰醋酸调节pH值后得到溶液B,将溶液A滴加到溶液B中,滴加过程中不断搅拌,陈化后得到溶胶,其中钛酸丁酯的用量为5mol,无水乙醇的用量为40mol,蒸馏水的用量为4mol,冰醋酸的用量为3.5mol,陈化时间为12h;
E.通过提拉法制备二氧化钛陶瓷薄膜,以5cm/min提拉速度涂覆上述溶胶,而后分别在80℃下干燥20min,在45℃下干燥20min,在25℃下干燥30min,自然冷却到室温,在300℃下烧结30min,烧结后根据薄膜厚度多次涂膜,最后在450℃下退火1h,得到厚度为3μm的二氧化钛陶瓷薄膜。
以下,通过溶血试验评价各样品的血液相容性,其原理在于:将样品与血液直接接触,测定红细胞膜破裂后释放的血红蛋白量,以检测各样品体外溶血程度。血红蛋白的吸收波长为545nm,可用分光光度计检测其浓度。具体操作步骤如下:
(1)从健康家兔心脏采血100mL,加入2%草酸钾5mL,制成新鲜抗凝血。取抗凝血40mL,加入0.9%氯化钠注射液50mL进行稀释。
(2)取3支硅化试管,一支试管装入试验样品和氯化钠注射液10mL,一支试管空白作为阴性对照组加入氯化钠生理盐水10mL,另外一支试管空白作为阳性对照组分别加入10mL蒸馏水。
(3)所有试管在37℃水浴中恒温30min,分别加入5mL抗凝兔血,并在37℃条件下保温60min。
(4)取试管上层清液,在545nm波长处测定吸光度。每一样品进行三次平行试验并取平均值。
溶血率的计算公式如下:
溶血率(%)=(试样平均吸光度-阴性组吸光度)/(阳性组吸光度-阴性组吸光度)×100
实施例1-4(对应A、B、C、D)及对比例1-3(对应X、Y、Z)的试验样品对应的溶血率如表1所示。
表1 实施例1-4以及对比例1-3的溶血实验数据
编号 | A | B | C | D | X | Y | Z |
溶血率/% | 5.4 | 2.1 | 6.3 | 9.2 | 15.7 | 16.3 | 19.2 |
从表1可以看出,在二氧化钛陶瓷薄膜中掺入石墨烯都有利于提高其血液相容性,但是掺入量过少或过多对于相容性性能的提高都不明显,在掺入量为5%-10.8%时,能够使得血管支架表面二氧化钛陶瓷薄膜的溶血率低于10%,在掺入量为7.3%时,更能使溶血率低至2.1%。
值得一提的时,上述实验数据旨在对比石墨烯的掺入对于二氧化钛陶瓷薄膜血液相容性的影响,以兔血为实验对象的溶血率实验不代表上述样品在人体的溶血率数据。
以上所述仅是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明技术原理的前提下,还可以做出若干改进和变型,这些改进和变型也应视为本发明的保护范围。
Claims (5)
1.一种溶胶-凝胶法制备掺杂二氧化钛陶瓷薄膜的方法,包括以下步骤:
A.以血管支架材料为衬底,所述血管支架材料为医用镁合金;
B.对衬底进行预处理,预处理包括脱脂、打磨、清洗和烘干,其中脱脂选用碳酸钠溶液,清洗选用无水乙醇并配合超声波辅助;
C.制备MgO过渡层:将烘干的衬底放入溅射镀膜设备中,以MgO靶为溅射源,在氩气气氛下制备MgO过渡层,其中电源功率为60-80W,氩气流量60-90sccm,衬底温度150-180℃,溅射时间18-30min;
D.将钛酸丁酯和无水乙醇混合得到溶液A,以无水乙醇和蒸馏水混合并添加石墨烯得到石墨烯分散液,用冰醋酸调节pH值后得到溶液B,将溶液A滴加到溶液B中,滴加过程中不断搅拌,陈化后得到溶胶,其中钛酸丁酯的用量为5-8mol,无水乙醇的用量为40-50mol,蒸馏水的用量为4-10mol,冰醋酸的用量为3.5-5mol,陈化时间为12-24h;
E.通过提拉法制备石墨烯掺杂二氧化钛陶瓷薄膜,以5-8cm/min提拉速度涂覆上述溶胶,而后分别在80-90℃下干燥20-25min,在45-50℃下干燥20-30min,在25-30℃下干燥30-50min,自然冷却到室温,在300-350℃下烧结30-40min,烧结后根据薄膜厚度多次涂膜,最后在450-500℃下退火1-2h,得到厚度为3-5μm的石墨烯掺杂二氧化钛陶瓷薄膜。
2.一种如权利要求1所述的方法,其特征在于:所述衬底为10×10*1.5mm的基片。
3.一种如权利要求1所述的方法,其特征在于:所述碳酸钠溶液的浓度为20-30wt%。
4.一种如权利要求1所述的方法,其特征在于:所述石墨烯的用量为整个溶胶质量的5%-10.8%。
5.一种如权利要求1所述的方法,其特征在于,所述石墨烯的用量为整个溶胶质量的7.3%。
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