CN110257807B - 一种纸基钯-氧化锌-金复合材料的制备方法 - Google Patents
一种纸基钯-氧化锌-金复合材料的制备方法 Download PDFInfo
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- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 14
- 239000011701 zinc Substances 0.000 title claims abstract description 14
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 52
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 50
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- 229910021607 Silver chloride Inorganic materials 0.000 claims description 6
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Abstract
本发明公开了一种纸基钯‑氧化锌‑金复合材料的制备方法,首先利用原位还原法在纸纤维表面包覆一层钯纳米粒子,获得纸基钯电极;然后通过电沉积法在纸基钯电极上生长氧化锌纳米棒;最后基于光协助的电沉积法在氧化锌纳米棒之间生长金纳米线,获得纸基钯‑氧化锌‑金复合材料。氧化锌纳米棒之间的金纳米线可以加速棒与棒之间的电子传递,同时电子沿着纳米棒向纸纤维网络表面的钯纳米粒子传递,形成三维的导电网络;该纸基复合材料不仅具有良好的导电性而且具有大的表面积,可以广泛地用于电化学、光电化学以及电化学发光传感分析领域。
Description
技术领域
本发明涉及复合纳米材料制备技术和纸芯片技术领域,更具体地说是一种纸基钯-氧化锌-金复合材料的制备方法。
背景技术
纸在日常生活中无处不在,其具有成本低、生物相容性好、便携、来源丰富等优点。纸自身纵横交错的纤维网络,使其具有大的表面积,有利于功能化大量的纳米材料,获得高性能的纸基复合材料。由于纸纤维具有较差的导电性,通常需要功能化贵金属、碳材料等增强其导电性。
氧化锌作为一种性能优异的半导体材料广泛地应用于电化学、光电化学、电化学发光等传感分析领域。氧化锌具有各种各样的形貌,比如纳米花、纳米片、纳米棒。氧化锌纳米棒自身独特的棒状结构可以加速电子沿着纳米棒传递,增强其导电性,但是棒与棒之间无法进行电子传递,为了更好地增强其导电性,进一步提高应用性能,需要在棒与棒之间功能化导电材料。
发明内容
本发明的目的是利用原位还原法在纸纤维上包覆钯纳米粒子层,获得具有良好的导电性和大的表面积的纸基钯电极,然后利用电沉积法在钯纳米粒子层上生长氧化锌纳米棒,最后利用光协助的电沉积法在获得的氧化锌纳米棒之间生长金纳米线,获得纸基钯-氧化锌-金复合材料。
一种纸基钯-氧化锌-金复合材料的制备方法具体包括如下步骤:
(1)首先利用计算机软件Adobe illustrator CS6设计纸芯片的形状和功能区以及相应的疏水蜡打印图案,然后通过蜡打印机将疏水蜡打印图案打印在色谱纸上,并在130℃条件下加热50 s,使蜡熔化并完全渗透到纸纤维中,所设计的纸芯片形状为边长为25 mm的正方形,中间未打蜡的直径为10 mm的圆形区域为亲水区域,周围的区域为打蜡的疏水区域,最后利用丝网印刷技术在纸芯片的亲水区域和疏水区域印刷一个长为13 mm,宽为5 mm的长方形碳导线;
(2)在纸芯片的亲水区域利用原位还原法生长钯纳米粒子层,将30-50 μL浓度为60-80 mM的氯钯酸溶液滴加到步骤(1)中获得的纸芯片的亲水区域,在4 ℃条件下静置10-30 min后,滴加30-50 μL 浓度为100-200 mM的抗坏血酸溶液,所用的抗坏血酸溶液提前在冰浴条件下处理10 min,继续在4 ℃条件下反应30-50 min,用二次水洗涤除去未反应的试剂,获得纸基钯电极;
(3)以步骤(2)中获得的纸基钯电极作为工作电极,铂电极作为对电极,Ag/AgCl电极作为参比电极,利用电沉积法在纸基钯电极表面电沉积氧化锌纳米棒,所用的电沉积溶液由浓度为0.5-2.0 M的氯化钾和浓度为0.01-0.03 M的硝酸锌组成,电沉积电压为-0.8 --1.6 V,电沉积时间为2-4 h,电沉积温度为50-70 ℃,电沉积完成后,氧化锌纳米棒生长在纸基钯电极表面,获得纸基钯-氧化锌电极;
(4)利用由铂对电极、Ag/AgCl参比电极及步骤(3)中获得的纸基钯-氧化锌电极组成的三电极系统,通过光协助的电沉积法在步骤(3)中获得的氧化锌纳米棒之间生长金纳米线,电沉积溶液为由氯金酸、聚乙烯比咯烷酮及磷酸钠组成的混合液,所用的氯金酸浓度为0.1-0.5 mM,聚乙烯比咯烷酮浓度为0.2-0.4 M,磷酸钠浓度为0.1-0.3 M,电沉积电压为-0.2 - -0.8 V,在光照射下电沉积时间为2-5 min,所用的照射光源为300 W的氙灯,沉积完成后,用二次水和无水乙醇依次洗涤电极表面,并在室温下自然干燥,获得纸基钯-氧化锌-金复合材料。
本发明的有益效果:
(1)制备的纸基钯-氧化锌-金复合材料不仅具有大的表面积而且具有良好的导电性,氧化锌纳米棒之间的金纳米线可以加速棒与棒之间的电子传递,同时电子沿着纳米棒向纸纤维网络表面的钯纳米粒子传递,形成三维的导电网络,其作为性能优异的纸基电极,具有较高的应用价值。
(2)联合原位还原法和电沉积法制备纸基钯-氧化锌-金复合材料,该方法操作简单、原材料来源丰富、成本低,适合大规模生产,具有较高的生产价值。
具体实施方式
为了更好地理解本发明,下面结合实施例进一步阐明本发明的内容,但本发明的内容不仅仅局限于下面的实施例。
实施例1
一种纸基钯-氧化锌-金复合材料的制备方法,具体制备方案如下:
(1)首先利用计算机软件Adobe illustrator CS6设计纸芯片的形状和功能区以及相应的疏水蜡打印图案,然后通过蜡打印机将疏水蜡打印图案打印在色谱纸上,并在130℃条件下加热50 s,使蜡熔化并完全渗透到纸纤维中,所设计的纸芯片形状为边长为25 mm的正方形,中间未打蜡的直径为10 mm的圆形区域为亲水区域,周围的区域为打蜡的疏水区域,最后利用丝网印刷技术在纸芯片的亲水区域和疏水区域印刷一个长为13 mm,宽为5 mm的长方形碳导线;
(2)在纸芯片的亲水区域利用原位还原法生长钯纳米粒子层,将40 μL浓度为70mM的氯钯酸溶液滴加到步骤(1)中获得的纸芯片的亲水区域,在4 ℃条件下静置20 min后,滴加40 μL 浓度为150 mM的抗坏血酸溶液,所用的抗坏血酸溶液提前在冰浴条件下处理10min,继续在4 ℃条件下反应30 min,用二次水洗涤除去未反应的试剂,获得纸基钯电极;
(3)以步骤(2)中获得的纸基钯电极作为工作电极,铂电极作为对电极,Ag/AgCl电极作为参比电极,利用电沉积法在纸基钯电极表面电沉积氧化锌纳米棒,所用的电沉积溶液由浓度为0.1 M的氯化钾和浓度为0.01 M的硝酸锌组成,电沉积电压为-1.1 V,电沉积时间为3 h,电沉积温度为70 ℃,电沉积完成后,氧化锌纳米棒生长在纸基钯电极表面,获得纸基钯-氧化锌电极;
(4)利用由铂对电极、Ag/AgCl参比电极及步骤(3)中获得的纸基钯-氧化锌电极组成的三电极系统,通过光协助的电沉积法在步骤(3)中获得的氧化锌纳米棒之间生长金纳米线,电沉积溶液为由氯金酸、聚乙烯比咯烷酮及磷酸钠组成的混合液,所用的氯金酸浓度为0.4 mM,聚乙烯比咯烷酮浓度为0.3 M,磷酸钠浓度为0.1 M,电沉积电压为-0.4 V,在光照射下电沉积时间为3 min,所用的照射光源为300 W的氙灯,沉积完成后,用二次水和无水乙醇依次洗涤电极表面,并在室温下自然干燥,获得纸基钯-氧化锌-金复合材料。
实施例2
制备步骤同例1,不同之处是:步骤(2)中在纸芯片的亲水区域利用原位还原法生长钯纳米粒子层,所用的氯钯酸溶液浓度为80 mM,抗坏血酸溶液浓度为200 mM。
实施例3
制备步骤同例1,不同之处是:步骤(3)中利用电沉积法在纸基钯电极表面电沉积氧化锌纳米棒,所用的电沉积溶液由浓度为2.0 M的氯化钾和浓度为0.03 M的硝酸锌组成。
实施例4
制备步骤同例1,不同之处是:步骤(3)中利用电沉积法在纸基钯电极表面电沉积氧化锌纳米棒,所述的电沉积电压为-0.8 V。
实施例5
制备步骤同例1,不同之处是:步骤(4)中通过光协助的电沉积法在步骤(3)中获得的氧化锌纳米棒之间生长金纳米线,所述的在光照射下电沉积时间为5 min。
实施例6
制备步骤同例1,不同之处是:步骤(4)中通过光协助的电沉积法在步骤(3)中获得的氧化锌纳米棒之间生长金纳米线,所用的氯金酸浓度为0.5 mM,聚乙烯比咯烷酮浓度为0.4 M,磷酸钠浓度为0.3 M。
Claims (1)
1.一种纸基钯-氧化锌-金复合材料的制备方法,其特征是包括以下步骤:
(1)首先利用计算机软件Adobe illustrator CS6设计纸芯片的形状和功能区以及相应的疏水蜡打印图案,然后通过蜡打印机将疏水蜡打印图案打印在色谱纸上,并在130 ℃条件下加热50 s,使蜡熔化并完全渗透到纸纤维中,所设计的纸芯片形状为边长为25 mm的正方形,中间未打蜡的直径为10 mm的圆形区域为亲水区域,周围的区域为打蜡的疏水区域,最后利用丝网印刷技术在纸芯片的亲水区域和疏水区域印刷一个长为13 mm,宽为5 mm的长方形碳导线;
(2)在纸芯片的亲水区域利用原位还原法生长钯纳米粒子层,将30-50 μL浓度为60-80mM的氯钯酸溶液滴加到步骤(1)中获得的纸芯片的亲水区域,在4 ℃条件下静置10-30 min后,滴加30-50 μL 浓度为100-200 mM的抗坏血酸溶液,所用的抗坏血酸溶液提前在冰浴条件下处理10 min,继续在4 ℃条件下反应30-50 min,用二次水洗涤除去未反应的试剂,获得纸基钯电极;
(3)以步骤(2)中获得的纸基钯电极作为工作电极,铂电极作为对电极,Ag/AgCl电极作为参比电极,利用电沉积法在纸基钯电极表面电沉积氧化锌纳米棒,所用的电沉积溶液由浓度为0.5-2.0 M的氯化钾和浓度为0.01-0.03 M的硝酸锌组成,电沉积电压为-0.8 - -1.6 V,电沉积时间为2-4 h,电沉积温度为50-70 ℃,电沉积完成后,氧化锌纳米棒生长在纸基钯电极表面,获得纸基钯-氧化锌电极;
(4)利用由铂对电极、Ag/AgCl参比电极及步骤(3)中获得的纸基钯-氧化锌电极组成的三电极系统,通过光协助的电沉积法在步骤(3)中获得的氧化锌纳米棒之间生长金纳米线,电沉积溶液为由氯金酸、聚乙烯比咯烷酮及磷酸钠组成的混合液,所用的氯金酸浓度为0.1-0.5 mM,聚乙烯比咯烷酮浓度为0.2-0.4 M,磷酸钠浓度为0.1-0.3 M,电沉积电压为-0.2 - -0.8 V,在光照射下电沉积时间为2-5 min,所用的照射光源为300 W的氙灯,沉积完成后,用二次水和无水乙醇依次洗涤电极表面,并在室温下自然干燥,获得纸基钯-氧化锌-金复合材料。
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