CN106011829B - 一种抗菌不锈钢及其制备方法 - Google Patents

一种抗菌不锈钢及其制备方法 Download PDF

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CN106011829B
CN106011829B CN201610506516.2A CN201610506516A CN106011829B CN 106011829 B CN106011829 B CN 106011829B CN 201610506516 A CN201610506516 A CN 201610506516A CN 106011829 B CN106011829 B CN 106011829B
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詹玮婷
倪红卫
陈荣生
胡万培
刘伟
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Wuhan University of Science and Engineering WUSE
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Abstract

本发明具体涉及一种抗菌不锈钢及其制备方法。其技术方案是：在‑5~40℃条件下，将表面预处理的不锈钢置于多巴胺缓冲溶液中沉积0.1~72h，再置于含钛离子的溶液中沉积0.1~6h，然后置于含银离子的溶液中沉积0.1~6h，即得到抗菌不锈钢。其中：多巴胺溶液的浓度为0.01~1mol/L；含钛离子溶液的浓度为0.001~1mol/L；含银离子溶液的浓度为0.001~1mol/L。本发明工艺简单、环境友好和成本低廉；用该方法所制备的抗菌不锈钢的表面抗菌纳米膜层结构规整有序、与基材结合牢固、耐腐蚀性强和硬度高，有光照和无光照条件下均具有优良的抗菌性能。

Description

一种抗菌不锈钢及其制备方法
技术领域
本发明属于不锈钢材料领域。具体涉及一种抗菌不锈钢及其制备方法。
背景技术
不锈钢在日常生活中的应用十分广泛，它不仅光洁美观而且能够耐腐蚀并防锈。随着人们的健康意识和卫生防菌意识日益提高，具有防菌抗菌杀菌功能的抗菌不锈钢应运而生。从实际应用来看，抗菌不锈钢所利用的更多的是不锈钢表面的抗菌性能，而合金型抗菌不锈钢则是在不锈钢表面和内部都含有抗菌金属离子，这不仅造成一定的浪费，而且也增加了生产成本和技术要求，因此，表面抗菌不锈钢有着极大的应用前景和研究价值。然而，现有表面抗菌不锈钢技术存在如下问题：
一是抗菌效果滞后。一般需要达到12小时以上甚至24小时才开始杀菌，大大限制了不锈钢在公共卫生场所的应用。如“一种离子液体修饰的抗菌不锈钢材料的制备方法”(CN201410373147.5)专利技术，处理后的不锈钢在大肠杆菌培养液中抗菌12h后显现出比较明显的抑制效果。
二是抗菌条件有限。有些表面抗菌不锈钢需要紫外光辐照达到光催化抗菌效果，这不仅在公共场所难以满足要求，且在工业以及家用领域对人体将产生一定伤害，同时在无光条件下抗菌效果难以保持。
三是抗菌薄膜制备工艺存在缺陷。所制备的涂层过厚，与基材结合不牢固，容易剥落，同时薄膜表面结构不可控，纳米难以保持均匀，难以达到纳米尺寸效应。
发明内容
本发明旨在克服已有技术缺陷，目的是提供一种工艺简单、环境友好和成本低廉的抗菌不锈钢的制备方法；用该方法制备的抗菌不锈钢的表面抗菌纳米膜层结构规整有序、与基材结合牢固、耐腐蚀性强和硬度高，有光照和无光照条件下的抗菌性能优良。
为实现上述目的，本发明采用的技术方案是：在-5～40℃条件下，将表面预处理的不锈钢置于多巴胺缓冲溶液中沉积0.1～72h，再置于含钛离子的溶液中沉积0.1～6h，然后置于含银离子的溶液中沉积0.1～6h，即得到抗菌不锈钢。
所述多巴胺溶液的浓度为0.01～1mol/L，pH值为8～10；
所述含钛离子溶液的浓度为0.001～1mol/L，pH值为1～8；
所述含银离子溶液的浓度为0.001～1mol/L，pH值为4～8。
所述含钛离子溶液为氟钛酸铵溶液、硫酸钛溶液和四氯化钛溶液中的一种。
所述含银离子溶液为硫酸银溶液、硝酸银溶液和氯化银溶液中的一种。
所述表面预处理是：先将不锈钢表面打磨至粗糙度小于Ra10μm，再先后在无水乙醇和蒸馏水中超声清洗，吹干。
由于采用上述方案，本发明与现有技术相比，具有以下优点：
1)本发明的制备过程是在常温下进行，生产过程简单，制备周期短，能耗小；所需的仪器设备投资少，所用原料价格低廉，利用率高，没有环境污染，适于批量生产。
2)本发明采用的溶液浸置法属于非线性过程，可对大面积和形状复杂的不锈钢制品进行纳米化处理。
3)本发明制备的抗菌不锈钢基本不改变不锈钢的尺寸形状，能保持原有材料的尺寸精度和表面粗糙度。
本发明制备的抗菌不锈钢：经金相显微镜观察表明，不锈钢膜层非常平滑，无凸起或凹陷区域；采用干、湿胶带实验测定不锈钢表面纳米薄膜与基体的结合性能，结果表明，膜层与不锈钢基体结合非常牢固，无脱落现象；采用电化学工作站测量不锈钢耐腐蚀性能，结果表明，具有纳米孔阵列薄膜的不锈钢表面耐腐蚀性能与制备前的不锈钢耐腐蚀性能相比没有明显改变；经显微硬度计检测，其表面硬度与制备前的不锈钢的表面硬度相比没有明显改变。
4)本发明工艺参数可精确控制，通过改变反应时间、反应温度和溶液浓度，能调整纳米抗菌涂层的形貌、组成和微观结构，重复性好。
5)本发明所得纳米膜层保持在20nm左右，表面结合能大，与基材结合力强，且附着均匀牢固，无脱落现象，耐腐蚀性强。
6)本发明所得TiO2/Ag纳米复合结构在10nm以内，在有光和无光条件下，都可以极大地提高纳米薄膜的抗菌性能，并可控调整复合结构，分布规整有序，且不锈钢耐腐蚀性强和硬度高。
7)本发明所制备的抗菌不锈钢表面细菌培养时间为15min时，在可见光辐照下的抗菌率达到99％以上，在无光条件下的抗菌率达到95％以上；本发明所制备的抗菌不锈钢表面细菌培养时间为180min时，在可见光辐照下的抗菌率达到99％以上，在无光条件下的抗菌率达到99％以上。结果表明，所制备的抗菌不锈钢在有光照和无光照条件下，对细菌均有优良的抗菌性能。
所以，本发明工艺简单、环境友好和成本低廉；用该方法所制备的抗菌不锈钢的表面抗菌纳米膜层结构规整有序、与基材结合牢固、耐腐蚀性强和硬度高，有光照和无光照条件下均具有优良的抗菌性能。
具体实施方式
下面结合具有实施方式对本发明作进一步的描述，并非对其保护范围的限制。
为避免重复，先将本具体实施方式所涉及的技术参数统一描述如下，实施例中不再赘述：
所述表面预处理是：先将不锈钢表面打磨至粗糙度小于Ra10μm，再先后在无水乙醇和蒸馏水中超声清洗，吹干。
所述多巴胺溶液的浓度为0.01～1mol/L，pH值为8～10。
实施例1
一种抗菌不锈钢及其制备方法。在-5～10℃条件下，将表面预处理的不锈钢置于多巴胺缓冲溶液中沉积0.1～3h，再置于含钛离子的溶液中沉积0.1～1h，然后置于含银离子的溶液中沉积0.1～1h，即得到抗菌不锈钢。
所述含钛离子溶液的浓度为0.001～0.005mol/L，pH值为6～8。
所述含银离子溶液的浓度为0.001～0.005mol/L，pH值为6～8。
所述含钛离子溶液为氟钛酸铵溶液；所述含银离子溶液为硝酸银溶液。
实施例2
一种抗菌不锈钢及其制备方法。在10～25℃条件下，将表面预处理的不锈钢置于多巴胺缓冲溶液中沉积3～12h，再置于含钛离子的溶液中沉积1～3h，然后置于含银离子的溶液中沉积1～3h，即得到抗菌不锈钢。
所述含钛离子溶液的浓度为0.005～0.05mol/L，pH值为4～6。
所述含银离子溶液的浓度为0.005～0.05mol/L，pH值为4～6。
所述含钛离子溶液为硫酸钛溶液；所述含银离子溶液为硫酸银溶液。
实施例3
一种抗菌不锈钢及其制备方法。在15～30℃条件下，将表面预处理的不锈钢置于多巴胺缓冲溶液中沉积12～36h，再置于含钛离子的溶液中沉积3～5h，然后置于含银离子的溶液中沉积3～5h，即得到抗菌不锈钢。
所述含钛离子溶液的浓度为0.05～0.5mol/L，pH值为3～5。
所述含银离子溶液的浓度为0.05～0.5mol/L，pH值为3～5。
所述含钛离子溶液为四氯化钛溶液；所述含银离子溶液为氯化银溶液。
实施例4
一种抗菌不锈钢及其制备方法。在30～40℃条件下，将表面预处理的不锈钢置于多巴胺缓冲溶液中沉积36～72h，再置于含钛离子的溶液中沉积4～6h，然后置于含银离子的溶液中沉积4～6h，即得到抗菌不锈钢。
所述含钛离子溶液的浓度为0.5～1mol/L，pH值为1～3。
所述含银离子溶液的浓度为0.5～1mol/L，pH值为1～3。
所述含钛离子溶液为四氯化钛溶液；所述含银离子溶液为硝酸银溶液。
本具体实施方式与现有技术相比，具有以下优点：
1)本具体实施方式的制备过程在常温下进行，生产过程简单，制备周期短，能耗小；所需的仪器设备投资少；所用原料价格低廉，利用率高，没有环境污染，适于批量生产。
2)本具体实施方式采用的溶液浸置法属于非线性过程，可对大面积和形状复杂的不锈钢制品进行纳米化处理。
3)本具体实施方式制备的抗菌不锈钢基本不改变不锈钢的尺寸形状，能保持原有材料的尺寸精度和表面粗糙度。
本具体实施方式制备的抗菌不锈钢：经金相显微镜观察表明，不锈钢膜层非常平滑，无凸起或凹陷区域；采用干、湿胶带实验测定不锈钢表面纳米薄膜与基体的结合性能，结果表明，膜层与不锈钢基体结合非常牢固，无脱落现象；采用电化学工作站测量不锈钢耐腐蚀性能，结果表明，具有纳米孔阵列薄膜的不锈钢表面耐腐蚀性能与制备前的不锈钢耐腐蚀性能相比没有明显改变；经显微硬度计检测，其表面硬度与制备前的不锈钢的表面硬度相比没有明显改变。
4)本具体实施方式工艺参数可精确控制，通过改变反应时间、反应温度和溶液浓度，能调整纳米抗菌涂层的形貌、组成和微观结构，重复性好。
5)本具体实施方式所得纳米膜层保持在20nm左右，表面结合能大，与基材结合力强，且附着均匀牢固，无脱落现象，耐腐蚀性强。
6)本具体实施方式所得TiO2/Ag纳米复合结构在10nm以内，在有光和无光条件下，都可以极大地提高纳米薄膜的抗菌性能，并可控调整复合结构，分布规整有序，且不锈钢耐腐蚀性强和硬度高。
7)本具体实施方式所制备的抗菌不锈钢表面细菌培养时间为15min时：在可见光辐照下的抗菌率达到99％以上，在无光条件下的抗菌率达到95％以上；本具体实施方式所制备的抗菌不锈钢表面细菌培养时间为180min时，在可见光辐照下的抗菌率达到99％以上，在无光条件下的抗菌率达到99％以上。结果表明，所制备的抗菌不锈钢在有光照和无光照条件下，对细菌均有优良的抗菌性能。
因此，本具体实施方式工艺简单、环境友好和成本低廉；用该方法所制备的抗菌不锈钢的表面抗菌纳米膜层结构规整有序、与基材结合牢固、耐腐蚀性强和硬度高，有光照和无光照条件下均具有优良的抗菌性能。

Claims (5)

1.一种抗菌不锈钢的制备方法，其特征在于所述制备方法是：在-5～40℃条件下，将表面预处理的不锈钢置于多巴胺缓冲溶液中沉积0.1～72h，再置于含钛离子的溶液中沉积0.1～6h，然后置于含银离子的溶液中沉积0.1～6h，即得到抗菌不锈钢；
所述多巴胺溶液的浓度为0.01～1mol/L，pH值为8～10；
所述含钛离子溶液的浓度为0.001～1mol/L，pH值为1～8；
所述含银离子溶液的浓度为0.001～1mol/L，pH值为4～8。
2.如权利要求1所述的抗菌不锈钢的制备方法，其特征在于所述含钛离子溶液为氟钛酸铵溶液、硫酸钛溶液和四氯化钛溶液中的一种。
3.如权利要求1所述的抗菌不锈钢的制备方法，其特征在于所述含银离子溶液为硫酸银溶液、硝酸银溶液和氯化银溶液中的一种。
4.如权利要求1所述的抗菌不锈钢的制备方法，其特征在于所述表面预处理是：先将不锈钢表面打磨至粗糙度小于Ra10μm，再先后在无水乙醇和蒸馏水中超声清洗，吹干。
5.一种抗菌不锈钢，其特征在于所述抗菌不锈钢是根据权利要求1～4项中任一项所述的抗菌不锈钢的制备方法所制备的抗菌不锈钢。
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