CN106967976B - 一种医用316L不锈钢表面二维有序纳米Se点阵的制备方法 - Google Patents
一种医用316L不锈钢表面二维有序纳米Se点阵的制备方法 Download PDFInfo
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Abstract
本发明涉及一种医用316L不锈钢表面二维有序纳米Se点阵的制备方法,包括:(1)将316LSS置于高氯酸的乙二醇电解液中,阳极氧化,得到具有纳米凹坑阵列的316LSS;2)将亚硒酸或亚硒酸盐溶液在搅拌下滴加到抗坏血酸溶液中,搅拌,得到Se溶液;(3)将步骤(2)中的Se溶液滴入到步骤(1)中的具有纳米凹坑阵列的316LSS中,‑5℃~10℃静置4~24h,清洗,干燥,煅烧即得。本发明解决了制备有序纳米Se点阵的问题,制备方法简单高效,环境友好,成本低廉;得到的Se纳米点阵粒径均一且分布规整,纳米Se点阵结构长程有序且分布密集,可用于材料表面功能改性和抗菌抗肿瘤等生物医药领域。
Description
技术领域
本发明属于316LSS材料领域,特别涉及一种医用316L不锈钢表面二维有序纳米Se点阵的制备方法。
背景技术
316LSS因其优良的性能和低廉的价格而广泛应用于临床医疗领域,在其长期临床应用中,仍然存在难以避免的问题和不足,如不具备生物活性和抗菌抗肿瘤等性能。为了赋予316LSS生物活性并改善其抗菌抗肿瘤性能,一种有效的方法就是对基体材料进行表面改性。
Se元素是人体必须的微量元素,参与机体正常的新陈代谢。纳米Se具有毒性弱、抗氧化性能好、生物活性高等优点,能保护生物体与细胞的氧化性损伤、调节自身免疫能力、增强药物协同性,是医学上用来预防和治疗疾病,维持生命健康的重要物质。有序的纳米Se点阵的比表面积大,具有更多的活性位点,从而赋予材料更优异的性能。此外,有序的纳米Se点阵可以提供一种物理凸起的结构,在细胞的生长过程中可以赋予其物理结构信号从而激活细胞内信号的通路,以达到促使细胞沿阵列的方向伸长生长的目的,这对研究细胞迁移、肿瘤发生等分子机理具有重要意义。
纳米硒的制备方法很多,专利201110117933.5公布了一种电化学法制备纳米硒的方法。专利201510597535.6公布过一种生物制备纳米硒的方法。但大多数制备工艺繁琐,体系复杂,能源消耗量大且未制备出尺寸均一的纳米硒。
最近,有关研究报道了通过氧化还原法在316LSS表面制备出纳米Se颗粒的方法(一种表面含纳米Se颗粒的316LSS的制备方法201510718220.2),其制备包括通过电化学阳极氧化法得到具有纳米坑阵列的316LSS并将其置于Se溶液中,得到Se/316LSS。该方法快速简便,可制得较小尺寸的纳米Se颗粒,但该方法制得的颗粒是无规分布在316LSS凹坑内,存在凹坑空填现象,且制备过程中纳米颗粒易团聚致使所得产物大小不均,可控度差,无法形成点阵结构。因此,要实现纳米Se有序点阵的制备,需要进一步的探索。
发明内容
本发明所要解决的技术问题是提供一种医用316L不锈钢表面二维有序纳米Se点阵的制备方法,该方法解决了制备有序纳米Se点阵的问题,制备方法简单高效,环境友好,成本低廉。
本发明的一种医用316L不锈钢表面二维有序纳米Se点阵的制备方法,包括:
(1)将316LSS置于高氯酸的乙二醇电解液中,阳极氧化,得到具有纳米凹坑阵列的316LSS;其中,高氯酸与乙二醇的体积比为1:15~25,电解液温度为-5℃~10℃;
(2)将亚硒酸或亚硒酸盐溶液在搅拌下滴加到抗坏血酸溶液中,搅拌,得到Se溶液;其中,亚硒酸或亚硒酸盐溶液与抗坏血酸溶液的体积比为1:1.5~4.5;
(3)将步骤(2)中的Se溶液滴入到步骤(1)中的具有纳米凹坑阵列的316LSS中,-5℃~10℃静置4~24h,清洗,干燥,煅烧得到表面具有有序纳米Se点阵的316LSS;其中,煅烧温度为250℃~550℃,升温速率为1℃/min~4℃/min,煅烧时间为3h~6h。
所述步骤(1)中的阳极氧化的电压为20V~70V,时间为30s~15min。
所述步骤(1)中的具有纳米凹坑阵列的316LSS表面坑径为50nm~150nm,表面坑深为2nm~9nm,表面坑密度为(1.5±0.3)×1010(个/cm2)。
所述步骤(2)中的亚硒酸盐为亚硒酸钠或亚硒酸钾。
所述步骤(2)中的亚硒酸或亚硒酸盐溶液的浓度为0.01mol/L~0.05mol/L,抗坏血酸溶液的浓度为0.01~0.1mol/L。
所述步骤(2)中的搅拌温度为0℃~10℃,时间为1min~10min。
所述步骤(3)中的清洗方式为用乙醇清洗后再用去离子水反复冲洗。
所述步骤(3)中的干燥温度为35℃~80℃,干燥时间为1h~10h。
所述步骤(3)中得到的表面具有有序纳米Se点阵的316LSS中Se纳米颗粒与316LSS基板之间的高度差为5nm~14nm。
所述Se纳米颗粒直径为40nm~140nm,间距为25nm~40nm,密度为(1.5±0.3)×1010(个/cm2)。
本发明首先采用氧化还原法制备纳米Se溶液,再以表面具有纳米坑阵列的316LSS作为载体,滴加纳米Se溶液,使溶液中的纳米Se颗粒均匀的分散在316LSS表面,随后将样品热处理,冷却后即得有序排布的纳米Se点阵。本发明操作便捷,高效温和,可制备出大面积二维有序纳米Se点阵,重复性好,具有广阔的应用前景。本发明利用表面改性技术弥补了316LSS不足并获得复合材料性能,具有重要的理论和应用价值。
本发明采用场发射扫描电镜(FESEM)观察316LSS表面纳米凹坑阵列,316LSS表面的纳米Se点阵表面形貌,采用X-射线能谱(EDS)分析材料表面元素组成的变化,其结果如图1~图4所示。
有益效果
(1)本发明的制备方法简单易行,环境友好,成本低廉且便于推广;
(2)本发明得到的纳米Se点阵高度有序,Se纳米颗粒粒径均一且分布规整;
(3)本发明得到的纳米Se点阵以316LSS表面的纳米凹坑阵结构为模板,复制出了与凹坑阵结构对应的有序凸点阵结构;
(4)本发明得到的纳米Se/316LSS具有显著的促ADSCs生长效应,可用于材料表面功能改性和抗菌抗肿瘤等生物医药领域。
附图说明
图1为实施例1中316LSS表面有序纳米凹坑阵列不同放大倍数下的FESEM图;
图2为实施例1中316LSS表面有序纳米Se阵列不同放大倍数下的FESEM图;
图3为实施例1中表面具有有序纳米坑阵列的316LSS的EDS能谱图;
图4为实施例1中316LSS表面有序纳米Se阵列的EDS能谱图;
图5为实施例1中316LSS表面有序纳米Se阵列的促ADSCs增长数据统计图。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。此外应理解,在阅读了本发明讲授的内容之后,本领域技术人员可以对本发明作各种改动或修改,这些等价形式同样落于本申请所附权利要求书所限定的范围。
实施例1
(1)316LSS表面纳米凹坑阵列的制备:将316LSS于高氯酸、乙二醇的混合液(V:V=1:15)中,体系溶液温度为0℃,40V阳极氧化10min,坑径为50nm,坑深为5nm,坑密度为1.5×1010(个/cm2)。
(2)Se溶液的制备:将0.1g的亚硒酸钠加入到10mL温度为3℃的去离子水中,搅拌均匀;将0.2g的抗坏血酸加入到20mL温度为3℃的去离子水中,搅拌均匀,然后保持温度为0℃边搅拌边将亚硒酸钠溶液滴加入抗坏血酸的水溶液中,时间为1min,得到Se溶液。
(3)将(2)中制得的Se溶液迅速滴入到装有纳米坑阵列的316LSS的玻璃小瓶中,5℃静置4h。
(4)取出样品,用乙醇和去离子水交替冲洗材料表面,在35℃下干燥6h。
(5)将样品在马弗炉中300℃焙烧,升温速率2℃/分钟,300℃下保温5h。
(6)将316LSS表面纳米Se点阵用FESEM和EDS进行表征,如图1、图2、图3和图4所示。其中,图1图2表明,利用316LSS的表面纳米坑阵列,制备了纳米颗粒有序点阵;图3和图4表明,316LSS表面的有序点阵是纳米Se阵列,其中,Se纳米颗粒直径为45nm,间距30nm,密度1.5×1010(个/cm2),Se纳米颗粒与316LSS基板之间的高度差为10nm。
(7)将未处理的316LSS、表面具有有序凹坑阵列的316LSS、纳米Se/316LSS用于ADSCs细胞增殖实验,其结果如图5所示。
促细胞生长的测试采用如下方法:实验细胞种类采用大鼠脂肪来源的P4代间充质干细胞(ADSCs),取对数生长期的细胞,调节细胞的浓度,使得细胞的密度为1×105个/孔,将细胞接种到事先加有灭菌过的未经处理的316LSS、表面具有纳米坑阵列316LSS以及纳米Se/316LSS的48孔板中,放入37℃、5%CO2培养箱中。为了定量比较细胞在各种材料上的粘附情况,分别在培养1d、3d、5d后取样进行细胞活性检测。具体测试步骤如下:在特定的时间点,取出种植有细胞的材料,置于新的48孔培养板中,用PBS轻轻漂洗材料以去除未贴附的细胞。每孔加入400μL事先配制好的CCK母液(含血清的DMEM培养液+10%CCK-8),放置于培养箱中继续培养,2h后,可肉眼观察到培养液变为金黄色,移走表面具有纳米坑阵列316LSS和纳米Se/316LSS,利用酶联免疫检测仪测定在波长为450nm处测定OD值。每次实验重复3次,每组样品设置5个复孔。在空白孔的培养基中加CCK-8,测定450nm的吸光度作为空白对照组。
由图5可知,316LSS表面的有序纳米Se点阵组的吸光度增长最为显著,其表面的Se点阵可促进ADSCs增殖,对ADSCs具有良好的细胞相容性。
实施例2
(1)316LSS表面纳米凹坑阵列的制备:将316LSS于高氯酸、乙二醇的混合液(V:V=1:19)中,体系溶液温度为2℃,40V阳极氧化11min,坑径为70nm,坑深7nm,坑密度为1.3×1010(个/cm2)。
(2)Se溶液的制备:将0.1g的亚硒酸钠加入到10mL温度为5℃的去离子水中,搅拌均匀;将0.3g的抗坏血酸加入到30mL温度为5℃的去离子水中,搅拌均匀,然后保持温度为2℃边搅拌边将亚硒酸钠溶液滴加入抗坏血酸的水溶液中,时间为1min,得到Se溶液。
(3)将(2)中制得的Se溶液迅速滴入到装有纳米凹坑阵列的316LSS的玻璃小瓶中,5℃静置18h。
(4)取出样品,用乙醇和去离子水交替冲洗材料表面,在60℃下干燥8h。
(5)将样品在马弗炉中350℃焙烧,升温速率2℃/分钟,350℃下保温3h。
(6)将316LSS表面纳米Se点阵用FESEM和EDS进行表征,结果与实施例1相似,其中,Se纳米颗粒直径为60nm,间距为30nm,密度为1.3×1010(个/cm2),Se纳米颗粒与316LSS基板之间的高度差为8nm。
(7)将未处理的316LSS、表面具有有序凹坑阵列的316LSS、纳米Se/316LSS用于ADSCs细胞增殖实验,结果与实施例1相似。
实施例3
(1)316LSS表面纳米凹坑阵的制备:将316LSS于高氯酸、乙二醇的混合液(V:V=1:25)中,体系溶液温度为0℃,70V阳极氧化30s,坑径为150nm,坑深为5nm,坑密度为1.2×1010(个/cm2)。
(2)Se溶液的制备:将0.1g的亚硒酸钠加入到10mL温度为8℃的去离子水中,搅拌均匀;将0.4g的抗坏血酸加入到40mL温度为8℃的去离子水中,搅拌均匀,然后保持温度为8℃边搅拌边将亚硒酸钠溶液滴加入抗坏血酸的水溶液中,时间为1min,得到Se溶液。
(3)将(2)中制得的Se溶液迅速滴入到装有纳米坑阵列的316LSS的玻璃小瓶中,8℃静置18h。
(4)取出样品,用乙醇和去离子水交替冲洗材料表面,在80℃下干燥1h。
(5)将样品在马弗炉中500℃焙烧,升温速率2℃/分钟,500℃下保温1.5h。
(6)将316LSS表面纳米Se点阵用FESEM和EDS进行表征,结果与实施例1相似,其中,Se纳米颗粒直径为140nm,间距为40nm,密度为1.2×1010(个/cm2),Se纳米颗粒与316LSS基板之间的高度差为5nm。
(7)将未处理的316LSS、表面具有有序坑阵列的316LSS、纳米Se/316LSS用于ADSCs细胞增殖实验,结果与实施例1相似。
Claims (1)
1.一种医用316L不锈钢表面二维有序纳米Se点阵的制备方法,包括:
(1)316LSS表面纳米凹坑阵列的制备:将316LSS于高氯酸、乙二醇的混合液(V:V=1:15)中,体系溶液温度为0℃,40V阳极氧化10min,坑径为50nm,坑深为5nm,坑密度为1.5×1010(个/cm2);
(2)Se溶液的制备:将0.1g的亚硒酸钠加入到10mL温度为3℃的去离子水中,搅拌均匀;将0.2g的抗坏血酸加入到20mL温度为3℃的去离子水中,搅拌均匀,然后保持温度为0℃边搅拌边将亚硒酸钠溶液滴加入抗坏血酸的水溶液中,时间为1min,得到Se溶液;
(3)将(2)中制得的Se溶液迅速滴入到装有纳米坑阵列的316LSS的玻璃小瓶中,5℃静置4h;
(4)取出样品,用乙醇和去离子水交替冲洗材料表面,在35℃下干燥6h;
(5)将样品在马弗炉中300℃焙烧,升温速率2℃/分钟,300℃下保温5h,得到具有有序纳米Se点阵的316LSS。
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CN105088304A (zh) * | 2015-08-10 | 2015-11-25 | 华南师范大学 | 一步模板法制备有序纳米点阵列的方法 |
CN105220203A (zh) * | 2015-10-29 | 2016-01-06 | 东华大学 | 一种316L不锈钢表面纳米SiO2点阵的制备方法 |
CN105256354A (zh) * | 2015-10-29 | 2016-01-20 | 东华大学 | 一种表面含纳米Se颗粒的316L不锈钢的制备方法 |
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CN105088304A (zh) * | 2015-08-10 | 2015-11-25 | 华南师范大学 | 一步模板法制备有序纳米点阵列的方法 |
CN105220203A (zh) * | 2015-10-29 | 2016-01-06 | 东华大学 | 一种316L不锈钢表面纳米SiO2点阵的制备方法 |
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