CN113373403B - 一种肠道支架表面气体渗氮的改性方法 - Google Patents
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Abstract
本发明涉及一种基于气体渗氮的表面改性方法,将镍钛合金肠道支架放在可分解的含氮气体中,其表面加热到高温时便能吸收初生氮或叫活性氮原子,这种活性氮原子被吸收并向深度扩散,进而对支架进行改性。氮原子的引入,提高了镍钛合金的耐腐蚀性能,与此相对应的是,镍钛合金的生物相容性却降低,通过控制气体氮化处理的时间,可以得到兼顾耐腐蚀性和生物相容性的肠道支架材料。
Description
技术领域
本发明涉及材料气体渗氮领域,具体涉及一种基于气体渗氮的表面改性方法。
背景技术
肠道支架植入术是指通过内镜检查找到肠道的狭窄段,并在内镜直视下将合适型号的类型的肠道支架经推送器送到狭窄的梗阻段并释放支架,使梗阻的肠管通畅。当肠道支架安置在肠道狭窄段后会自动膨胀,在人体体温的作用下,肠道支架会变得较硬且富有弹性,达到支撑肠腔的作用,同时,肠道支架能随肠道蠕动而呈现与肠道蠕动相适应的各种形态,使肠道保持长时间通畅,从而接触肠道梗阻。
对肠道支架而言,耐腐蚀性和生物相容性是最为关键的两种性能,耐腐蚀性能决定了支架材料的使用时长,而生物相容性则决定了支架材料对人体的副作用。由于肠道支架需要通过蠕动与肠道的蠕动相适应,因而通常的结构为网状。对于这种异形结构的支架材料而言,难以通过常用的镀覆工艺(如溅射法、热喷涂等)在其表面制备均匀分布的耐腐蚀改性涂层,并且,耐腐蚀改性涂层制备不当将降低支架材料的生物相容性。有鉴于此,如何得到耐腐蚀性和生物相容性都优异的肠道支架材料是当下急需解决的难题。
发明内容
针对现有技术存在的问题,本发明旨在提供一种基于气体渗氮的表面改性方法,用以提高现有镍钛合金肠道支架耐腐蚀的同时保持其优异的生物相容性。
一种基于气体渗氮的表面改性方法,其特征在于,包括以下步骤:
A.选用镍钛合金作为衬底材料,并将镍钛合金加工成网状结构;
B.将衬底材料先后放入碳酸钠溶液、丙酮和无水乙醇中进行脱脂处理;
C.将脱脂后的衬底材料放入HCl溶液中酸洗处理,以除去衬底表面的氧化层;
D.采用去离子水除去衬底表面残留的酸液,并在氮气条件下烘干待用;
E.将衬底放入气体渗氮炉中,通入氮气和氢气进行渗氮处理,渗氮过程中以20-25℃/min的升温速率先将温度升高至560-580℃,然后保温,最后随炉冷却。
进一步地,所述镍钛合金中钛和镍为等摩尔配比。
进一步地,所述碳酸钠溶液的浓度为15%。
进一步地,所述HCl溶液的浓度为10%。
进一步地,所述氮气和氢气的体积比为3∶1。
进一步地,所述保温时间为2-4h。
进一步地,所述保温时间为3.5h。
另外,本发明还提供了一种肠道支架,该支架由上述基于气体渗氮的表面改性方法制备而得。
镍钛合金肠道支架在可分解的含氮气体中,其表面加热到高温时便能吸收初生氮或叫活性氮原子,这种活性氮原子被吸收并向深度扩散,进而对支架进行改性。氮原子的引入,提高了镍钛合金的耐腐蚀性能,与此相对应的是,镍钛合金的生物相容性却降低,通过控制气体氮化处理的时间,可以得到兼顾耐腐蚀性和生物相容性的肠道支架材料。
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
A.选用镍钛合金作为衬底材料,并将镍钛合金加工成网状结构,其中钛和镍为等摩尔配比;
B.将衬底材料先后放入碳酸钠溶液、丙酮和无水乙醇中进行脱脂处理,其中碳酸钠溶液的浓度为15%;
C.将脱脂后的衬底材料放入HCl溶液中酸洗处理,以除去衬底表面的氧化层,其中HCl溶液的浓度为10%;
D.采用去离子水除去衬底表面残留的酸液,并在氮气条件下烘干待用;
E.将衬底放入气体渗氮炉中,通入氮气和氢气进行渗氮处理,渗氮过程中以20℃/min的升温速率先将温度升高至560℃,保温2h,然后随炉冷却,氮气和氢气的体积比为3∶1。
实施例2
A.选用镍钛合金作为衬底材料,并将镍钛合金加工成网状结构,其中钛和镍为等摩尔配比;
B.将衬底材料先后放入碳酸钠溶液、丙酮和无水乙醇中进行脱脂处理,其中碳酸钠溶液的浓度为15%;
C.将脱脂后的衬底材料放入HCl溶液中酸洗处理,以除去衬底表面的氧化层,其中HCl溶液的浓度为10%;
D.采用去离子水除去衬底表面残留的酸液,并在氮气条件下烘干待用;
E.将衬底放入气体渗氮炉中,通入氮气和氢气进行渗氮处理,渗氮过程中以20℃/min的升温速率先将温度升高至560℃,保温2.5h,然后随炉冷却,氮气和氢气的体积比为3∶1。
实施例3
A.选用镍钛合金作为衬底材料,并将镍钛合金加工成网状结构,其中钛和镍为等摩尔配比;
B.将衬底材料先后放入碳酸钠溶液、丙酮和无水乙醇中进行脱脂处理,其中碳酸钠溶液的浓度为15%;
C.将脱脂后的衬底材料放入HCl溶液中酸洗处理,以除去衬底表面的氧化层,其中HCl溶液的浓度为10%;
D.采用去离子水除去衬底表面残留的酸液,并在氮气条件下烘干待用;
E.将衬底放入气体渗氮炉中,通入氮气和氢气进行渗氮处理,渗氮过程中以20℃/min的升温速率先将温度升高至560℃,保温3.0h,然后随炉冷却,氮气和氢气的体积比为3∶1。
实施例4
A.选用镍钛合金作为衬底材料,并将镍钛合金加工成网状结构,其中钛和镍为等摩尔配比;
B.将衬底材料先后放入碳酸钠溶液、丙酮和无水乙醇中进行脱脂处理,其中碳酸钠溶液的浓度为15%;
C.将脱脂后的衬底材料放入HCl溶液中酸洗处理,以除去衬底表面的氧化层,其中HCl溶液的浓度为10%;
D.采用去离子水除去衬底表面残留的酸液,并在氮气条件下烘干待用;
E.将衬底放入气体渗氮炉中,通入氮气和氢气进行渗氮处理,渗氮过程中以20℃/min的升温速率先将温度升高至560℃,保温3.5h,然后随炉冷却,氮气和氢气的体积比为3∶1。
实施例5
A.选用镍钛合金作为衬底材料,并将镍钛合金加工成网状结构,其中钛和镍为等摩尔配比;
B.将衬底材料先后放入碳酸钠溶液、丙酮和无水乙醇中进行脱脂处理,其中碳酸钠溶液的浓度为15%;
C.将脱脂后的衬底材料放入HCl溶液中酸洗处理,以除去衬底表面的氧化层,其中HCl溶液的浓度为10%;
D.采用去离子水除去衬底表面残留的酸液,并在氮气条件下烘干待用;
E.将衬底放入气体渗氮炉中,通入氮气和氢气进行渗氮处理,渗氮过程中以20℃/min的升温速率先将温度升高至560℃,保温4.0h,然后随炉冷却,氮气和氢气的体积比为3∶1。
对比例1
A.选用镍钛合金作为衬底材料,并将镍钛合金加工成网状结构,其中钛和镍为等摩尔配比;
B.将衬底材料先后放入碳酸钠溶液、丙酮和无水乙醇中进行脱脂处理,其中碳酸钠溶液的浓度为15%;
C.将脱脂后的衬底材料放入HCl溶液中酸洗处理,以除去衬底表面的氧化层,其中HCl溶液的浓度为10%;
D.采用去离子水除去衬底表面残留的酸液,并在氮气条件下烘干待用;
E.将衬底放入气体渗氮炉中,通入氮气和氢气进行渗氮处理,渗氮过程中以20℃/min的升温速率先将温度升高至560℃,保温0.5h,然后随炉冷却,氮气和氢气的体积比为3∶1。
对比例2
A.选用镍钛合金作为衬底材料,并将镍钛合金加工成网状结构,其中钛和镍为等摩尔配比;
B.将衬底材料先后放入碳酸钠溶液、丙酮和无水乙醇中进行脱脂处理,其中碳酸钠溶液的浓度为15%;
C.将脱脂后的衬底材料放入HCl溶液中酸洗处理,以除去衬底表面的氧化层,其中HCl溶液的浓度为10%;
D.采用去离子水除去衬底表面残留的酸液,并在氮气条件下烘干待用;
E.将衬底放入气体渗氮炉中,通入氮气和氢气进行渗氮处理,渗氮过程中以20℃/min的升温速率先将温度升高至560℃,保温8.0h,然后随炉冷却,
氮气和氢气的体积比为3∶1。
接下来,我们对以上各样品的耐腐蚀性能和生物相容性进行评判。
关于生物相容性,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
关于耐腐蚀性能,通过Tafel直线外推法进行测量,测量过程的腐蚀介质为磷酸盐缓冲液(PBS)。
另外,选择未进行渗氮处理的镍钛合金作为空白对照组。各实验样品的测试数据如表1所示。
表1 各样品相变含量
编号 | 自腐蚀电流密度/μA·cm<sup>-2</sup> | 溶血率/% |
实施例1 | 17.2 | 4.7 |
实施例2 | 12.3 | 4.9 |
实施例3 | 7.6 | 5.4 |
实施例4 | 5.5 | 5.3 |
实施例5 | 3.1 | 6.2 |
对比例1 | 45.3 | 3.9 |
对比例2 | 0.7 | 20.3 |
空白对照组 | 62.8 | 3.1 |
从表1可以看出,对镍钛合金进行气体渗氮处理可以显著降低其自腐蚀电流密度,进而提高其耐腐蚀性能,延长使用寿命,并且,随着渗氮处理时间的延长,其耐腐蚀性能越发优异,然而,长时间的渗氮处理会导致其生物相容性降低。溶血率低于10%定义为生物相容性合格,通过控制渗氮时间可以在提高镍钛合金肠道支架耐腐蚀性能的同时保持良好的生物相容性。
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 (6)
1.一种肠道支架表面气体渗氮的改性方法,其特征在于,包括以下步骤:
A.选用镍钛合金作为衬底材料,并将镍钛合金加工成网状结构;
B.将衬底材料先后放入碳酸钠溶液、丙酮和无水乙醇中进行脱脂处理;
C.将脱脂后的衬底材料放入HCl溶液中酸洗处理,以除去衬底表面的氧化层;
D.采用去离子水除去衬底表面残留的酸液,并在氮气条件下烘干待用;
E.将衬底放入气体渗氮炉中,通入氮气和氢气进行渗氮处理,渗氮过程中以20-25℃/min的升温速率先将温度升高至560-580℃,然后保温2-4h,最后随炉冷却。
2.一种如权利要求1所述的改性方法,其特征在于:所述镍钛合金中钛和镍为等摩尔配比。
3.一种如权利要求1所述的改性方法,其特征在于:所述碳酸钠溶液的浓度为15%。
4.一种如权利要求1所述的改性方法,其特征在于:所述HCl溶液的浓度为10%。
5.一种如权利要求1所述的改性方法,其特征在于:所述氮气和氢气的体积比为3∶1。
6.一种如权利要求1所述的改性方法,其特征在于:保温时间为3.5h。
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