CN106198659B - 一种在微流控孔道中沉积纳米金的方法 - Google Patents
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Abstract
本发明涉及一种在微流控孔道中沉积纳米金的方法。通过对ITO玻璃进行预处理,制备出带有(PDDA/PSS)n多层自组装膜的ITO玻璃,以该ITO玻璃为基底与由PDMS制成的芯片封接而形成微流控芯片,然后将KAuCl4和H2SO4混合液注入微流控孔道中,通过计时电流法在其中沉积纳米金,纳米金表面形貌检测显示在微流控孔道内可见分布均匀的纳米金颗粒。本发明具有快速、简单、重复性好、成本低等特点,在医学生物工程、医学生物传感器等领域有广阔的应用前景。
Description
技术领域
本发明涉及微流控孔道表面处理技术,具体涉及一种在微流控孔道中沉积纳米金的工艺方法。
背景技术
微流控也被称作微流控芯片或微流控实验室,通常指把生物医学和化学实验过程中的采样、样品预处理、进样、分离、检测等操作过程有效集中在一块几平方厘米大小的芯片上的一种技术平台[1]。微流控技术被广泛地应用与化学[2,3]及生物医学[4,5]等领域,极大地简化了操作步骤,缩短了反应时间,增强了检测灵敏度,提高了整体效率。纳米金是指金的粒径为1-100nm之间的粒子,通过修饰,纳米金可以和DNA、RNA、蛋白质等分子结合,应用于生物医学及生物传感器方面,汪毅等人[6]利用两组DNA探针修饰的纳米金微粒,有效地检测乙肝病毒DNA。薛瑞等人[7]利用层层自组装技术制作了生物传感器利用带正的高分子聚电解质聚二烯丙基二甲基氯化铵,把金纳米粒子和乙酰胆碱酯酶通过静电逐层固定至玻碳电极的表面,使得被固定的乙酰胆碱酯酶对其底物具有更快的响应度及更高的亲和力。因此,在微流控孔道中应用纳米金的生物反应活性,可以有效地拓展微流控的应用范围,将与纳米金的相关实验微型化。然而目前尚无在微流控孔道中对纳米金进行快速、简单、重复性好、低成本沉积的方法[8],严重制约了纳米金在微流控中的应用。
发明内容
本发明的目的在于克服现有技术的不足,提供一种以带有(PDDA/PSS)n多层自组装膜的ITO玻璃为基底,用KAuCl4和H2SO4混合液,采用计时电流法,在聚二甲基硅氧烷(PDMS)微流控孔道内进行纳米金沉积的方法,避免使用贵重仪器、复杂工艺条件等问题。
本发明通过以下技术方案予以实现:一种在微流控孔道中沉积纳米金的方法,包括以下步骤:
S1将PDMS单体和引发体按10:1的质量比制备成微流控芯片;
S2ITO玻璃经臭氧清洗,使其表面附带大量负电荷;
S3将经过臭氧处理后的ITO玻璃放入聚二烯丙基二甲基氯化铵(PDDA)溶液中形成多层PDDA层与聚苯乙烯磺酸钠(PSS)组装,制备出带有(PDDA/PSS)n多层自组装膜的ITO玻璃,n大于1;
S4在匀胶机中将光刻胶均匀地铺在S3处理过ITO玻璃上,将微流控芯片与ITO玻璃封接在一起;
S5采用三电极体系,将KAuCl4和H2SO4的混合液注入微流控通道中,采用计时电流法进行纳米金沉积。
优选地,所述步骤S2中,先用无水乙醇超声清洗ITO玻璃,再置于紫外臭氧清洗机中30min。
优选地,所述步骤S3中,PDDA溶液浓度为1~10mg/mL,优选1mg/mL。
优选地,所述步骤S5中三电极体系为:将表面带有(PDDA/PSS)n静电自组装层的ITO玻璃作为工作电极,铂片电极为对电极,Ag/AgCl电极为参比电极。
优选地,所述步骤S5中计时电流法中固定沉积电压为1~-1000mV,时间为1~3600s;具体数值要经测试后搭配使用,如当n=6时,优选固定沉积电压为-200mV,时间为200s。
优选地,所述步骤S5中,KAuCl4浓度为0.0001~1mol/L,H2SO4浓度为0.0001~1mol/L,具体数值要经测试后搭配使用,如当n=6时,优选KAuCl4浓度为0.1mol/L,H2SO4浓度为0.5mol/L。
与现有技术相比,本发明的有益效果是:
本发明以带有(PDDA/PSS)n多层自组装膜的ITO玻璃为基底与由PDMS制成的芯片封接而形成微流控芯片,然后将KAuCl4和H2SO4混合液注入微流控孔道中,通过计时电流法在其中沉积纳米金。由于ITO玻璃及PDMS价格低廉,所用的层层组装法及计时电流法简单易行,结果重复性高,非常适合在微流控孔道中制备稳定的纳米金沉积膜。纳米金表面形貌检测显示在微流控孔道内可见分布均匀的纳米金颗粒。本发明具有快速、简单、重复性好、成本低等特点,避免了使用昂贵的仪器、繁琐的工艺方法、苛刻的制备条件,将纳米金沉积在微流控孔道中,在生物医学检测及生物传感器领域有着广泛的应用价值及应用潜力。
附图说明
图1为本发明实施例1带有(PDDA/PSS)6多层自组装膜的ITO玻璃纳米金沉积前后的对比;
图2为本发明实施例1纳米金在微流控孔道中的沉积照片;
图3为本发明实施例1纳米金的电镜形貌表征照片。
具体实施方式
下述非限制性实施例可以使本领域的普通技术人员更全面地理解本发明,但不以任何方式限制本发明。下述实施例中如无特殊说明,所采用的实验方法均为常规方法,所用材料、试剂等均可从化学公司购买。PDMS可以采用本领域公知的任一种制备方法,其中单体和引发体购于Momentive公司,名称:RTV615044-PL BX Kit(分A、B液),货号:009482。
实施例1
(1)将PDMS A液(单体)和B液(引发体)按10:1的质量比倒入烧杯中,用玻璃棒搅拌5分钟后倒进上述装有硅片的培养皿中。
(2)将培养皿放于浓缩干燥器中,用隔膜真空泵抽气1.5小时以除去PDMS中的气泡,然后置于80℃的真空干燥箱固化1小时。
(3)待其自然冷却后将PDMS从硅片模板上轻轻剥离,用切割机切成小块,再用手动芯片打孔机在相应部位打孔,以备实验使用。
(4)用无水乙醇超声清洗ITO玻璃,再置于紫外臭氧清洗机中30分钟,然后将清洗好的ITO的导电面朝上放置,放入1mg/mL的PDDA溶液中浸泡5min,取出后,使用蒸馏水少量多次进行清洗,然后使用氮气吹干。
(5)使用同样的步骤,对组装有PDDA层的ITO玻璃进行PSS组装。完成后,可制得一层(PDDA/PSS)自组装层。重复上述的过程6次,可制备出带有(PDDA/PSS)6多层自组装膜的ITO玻璃。
(6)最后用氮气封装在培养皿中待用。
(7)将事先准备好的ITO玻璃片放在匀胶机的转盘上,然后在硅片的中心加入200μL的PDMS,通过匀胶机将光刻胶均匀地铺满整个玻璃片表面。
(8)将打好孔的芯片在上述玻璃片上粘取PDMS,然后与ITO玻璃的导电面粘接在一起。
(9)准备好电化学工作站,采用三电极体系,表面带有(PDDA/PSS)6静电自组装层的ITO玻璃为工作电极,铂片电极为对电极,Ag/AgCl电极为参比电极。
(10)将KAuCl4(0.1mol/L)和H2SO4(0.5mol/L)混合液200μL注入微流控通道中,采用计时电流法,固定沉积电压为-200mV,采用200s的时间,进行纳米金沉积。带有(PDDA/PSS)6静电自组装层的ITO玻璃进行纳米金沉积后前后见图1,纳米金在微流控孔道中沉积前后如图2所示。通过扫描电子显微镜可以观察到微流控孔道中纳米金的形貌,见图3。
实施例2
(1)将PDMS A液(单体)和B液(引发体)按10:1的质量比倒入烧杯中,用玻璃棒搅拌5分钟后倒进上述装有硅片的培养皿中。将培养皿放于浓缩干燥器中,用隔膜真空泵抽气1.5小时以除去PDMS中的气泡,然后置于80℃的真空干燥箱固化1小时。待其自然冷却后将PDMS从硅片模板上轻轻剥离,用切割机切成小块,再用手动芯片打孔机在相应部位打孔,以备实验使用。
(2)用无水乙醇超声清洗ITO玻璃,再置于紫外臭氧清洗机中30分钟,然后将清洗好的ITO的导电面朝上放置,放入10mg/mL的PDDA溶液中浸泡5min,取出后,使用蒸馏水少量多次进行清洗,然后使用氮气吹干。使用同样的步骤,对组装有PDDA层的ITO玻璃进行PSS组装。完成后,可制得一层(PDDA/PSS)自组装层。重复上述的过程10次,可制备出带有(PDDA/PSS)10多层自组装膜的ITO玻璃。最后用氮气封装在培养皿中待用。
(3)将事先准备好的ITO玻璃片放在匀胶机的转盘上,然后在硅片的中心加入200μL的PDMS,通过匀胶机将光刻胶均匀地铺满整个玻璃片表面。将打好孔的芯片在上述玻璃片上粘取PDMS,然后与ITO玻璃的导电面粘接在一起。
(4)准备好电化学工作站,采用三电极体系,表面带有(PDDA/PSS)10静电自组装层的ITO玻璃为工作电极,铂片电极为对电极,Ag/AgCl电极为参比电极。将KAuCl4(0.2mol/L)和H2SO4(0.2mol/L)混合液200μL注入微流控通道中,采用计时电流法,固定沉积电压为-400mV,采用1600s的时间,进行纳米金沉积。
实施例3
(1)将PDMS A液(单体)和B液(引发体)按10:1的质量比倒入烧杯中,用玻璃棒搅拌5分钟后倒进上述装有硅片的培养皿中。将培养皿放于浓缩干燥器中,用隔膜真空泵抽气1.5小时以除去PDMS中的气泡,然后置于80℃的真空干燥箱固化1小时。待其自然冷却后将PDMS从硅片模板上轻轻剥离,用切割机切成小块,再用手动芯片打孔机在相应部位打孔,以备实验使用。
(2)用无水乙醇超声清洗ITO玻璃,再置于紫外臭氧清洗机中30分钟,然后将清洗好的ITO的导电面朝上放置,放入10mg/mL的PDDA溶液中浸泡5min,取出后,使用蒸馏水少量多次进行清洗,然后使用氮气吹干。使用同样的步骤,对组装有PDDA层的ITO玻璃进行PSS组装。(PDDA/PSS)在ITO玻璃上至少应形成1层膜,这样纳米银或纳米金才能在微流控孔道中沉积。完成后,可制得一层(PDDA/PSS)自组装层。重复上述的过程15次,可制备出带有(PDDA/PSS)15多层自组装膜的ITO玻璃。最后用氮气封装在培养皿中待用。
(3)将事先准备好的ITO玻璃片放在匀胶机的转盘上,然后在硅片的中心加入200μL的PDMS,通过匀胶机将光刻胶均匀地铺满整个玻璃片表面。将打好孔的芯片在上述玻璃片上粘取PDMS,然后与ITO玻璃的导电面粘接在一起。
(4)准备好电化学工作站,采用三电极体系,表面带有(PDDA/PSS)15静电自组装层的ITO玻璃为工作电极,铂片电极为对电极,Ag/AgCl电极为参比电极。将KAuCl4(1mol/L)和H2SO4(1mol/L)混合液200μL注入微流控通道中,采用计时电流法,固定沉积电压为-600mV,采用200s的时间,进行纳米金沉积。
以上所述,仅为本发明创造较佳的具体实施方式,但本发明创造的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明创造披露的技术范围内,根据本发明创造的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明创造的保护范围之内。
参考文献
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[3]彭金兰,徐溢,吴永杰,等.微流控芯片上大肠杆菌的电化学阻抗检测方法研究[J].分析化学研究报告,2011,39(9):1307-1312.
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[5]徐征,陆佳庆,Morimoto Ryo,等.基于微流控芯片的尿酸和抗坏血酸并行电化学检测研究[J].传感技术学报,2015,28(8):1103-1107.
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Claims (1)
1.一种在微流控孔道中沉积纳米金的方法,其特征在于,包括以下步骤:
S1.将PDMS单体和引发体按10:1的质量比制备成微流控芯片:
(1)将PDMS单体和引发体按10:1的质量比倒入烧杯中,用玻璃棒搅拌5分钟后倒进装有硅片的培养皿中;
(2)将培养皿放于浓缩干燥器中,用隔膜真空泵抽气1.5小时除去PDMS中的气泡,然后置于80℃的真空干燥箱固化1小时;
(3)待其自然冷却后将PDMS从硅片模板上轻轻剥离,用切割机切成小块,再用手动芯片打孔机在相应部位打孔,制备成微流控芯片;
S2.ITO玻璃经臭氧清洗,使其表面附带大量负电荷;
S3.将经过臭氧处理后的ITO玻璃放入浓度为1mg/mLPDDA溶液中与PSS组装,制备出带有(PDDA/PSS)n多层自组装膜的ITO玻璃,n=6;
步骤S2、S3的具体步骤是:
(4)用无水乙醇超声清洗ITO玻璃,再置于紫外臭氧清洗机中30分钟,然后将清洗好的ITO的导电面朝上放置,放入1mg/mL的PDDA溶液中浸泡5min,取出后,使用蒸馏水少量多次进行清洗,然后使用氮气吹干;
(5)对组装有PDDA层的ITO玻璃进行PSS组装,完成后,可制得一层(PDDA/PSS)自组装层,重复上述的过程6次,制备出带有(PDDA/PSS)6多层自组装膜的ITO玻璃;
(6)最后用氮气封装在培养皿中待用;
S4.在匀胶机中将光刻胶均匀地铺在S3处理过的ITO玻璃上,将微流控芯片与ITO玻璃封接在一起;
步骤S4的具体步骤是:
(7)将事先准备好的ITO玻璃放在匀胶机的转盘上,然后在硅片的中心加入200μL的PDMS,通过匀胶机将光刻胶均匀地铺满整个ITO玻璃表面;
(8)在上述ITO玻璃上将打好孔的微流控芯片粘取PDMS,然后与ITO玻璃的导电面粘接在一起;
S5.采用三电极体系,将表面带有(PDDA/PSS)6静电自组装膜的ITO玻璃作为工作电极,铂片电极为对电极,Ag/AgCl电极为参比电极;将浓度为0.1mol/LKAuCl4和浓度为0.5mol/LH2SO4的混合液注入微流控孔道中,采用计时电流法进行纳米金沉积,固定沉积电压为1~-1000mV,时间为1~3600s,带有(PDDA/PSS)6静电自组装膜的ITO玻璃进行纳米金沉积,纳米金在微流控孔道中沉积。
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