微通道内表面的微/纳米结构构筑及功能化设计
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摘要
微流控技术作为当今世界上最前沿的科技领域之一,凭借其高通量、低消耗的技术优势,在生命科学和工业合成等领域显示出了巨大的应用前景。微通道作为微流控芯片的重要组成部分,在该领域发展的初期,其内表面只是一个提供微空间的纯表面,而随着微流控技术的发展,尤其是微流控芯片在生物检测方面各种各样的具体应用,势必要求对微通道内表面进行必要的改性以满足不同的需求。与简单地在内表面制备一层功能膜相比,对微通道的内表面进行几何结构修饰,即在微通道内表面上构筑一些精细的微/纳米结构,并在这些微/纳米结构上再嫁接功能基团或分子,显然能够使微通道内表面具有更多的功能,是促进微通道内表面器件化和微流控技术进步的一个重要研究方向。目前在开放的微通道表面上构筑微/纳米结构的微细加工(microfabrication)技术主要有刻蚀技术、光刻法、软光刻法、LIGA技术等,然而这些方法都难以在细长的、几乎封闭的微通道内使用,而且开放微通道的封接过程势必会造成对已形成的微/纳米结构的破坏。鉴于此,本文用湿化学的方法在几乎封闭的石英毛细管微通道中构筑特定的微/纳米结构,并对已构筑的微/纳米结构进行表面改性赋予所设计的微流控器件特定的功能,成功设计出了微通道式光催化用微反应器和微蛋白分子富集器。将一维纳米材料的微/纳米结构直接集成到封闭的微通道中,避免了微通道传统微/纳米结构修饰过程中因封接带来的破坏,而且利用一维纳米材料器件化的最新研究成果,大大扩展了微流控器件的功能化设计。
利用湿化学的方法,借助纳米技术将ZnO纳米棒阵列和分布密度可控的ZnO纳米棒花状簇集成到了石英毛细管微流控通道的内表面上。利用NaOH和Zn(AC)2·2H2O的乙醇溶液在微通道内表面上制备了一层ZnO晶种膜；利用反相微乳液法和高温去乳化作用引起的晶粒团聚,在微通道内表面上得到了分散可控的ZnO晶种。晶种在基底上的分散性对于晶体的生长及最终形貌非常重要。在完全覆盖有一层ZnO晶种膜的微通道内表面上实现了ZnO纳米棒阵列的垂直生长；在分散可控的ZnO晶种基础上实现了分布密度可控的ZnO纳米棒花状簇的生长。研究发现,水与表面活性剂的摩尔比值w是影响晶种分散和纳米棒分布密度的主要因素,通过改变w值的大小改变了水滴的大小进而改变了颗粒大小,然后借助毛细管通道内表面对于不同尺寸纳米颗粒的粘附力不同,有效地调控了晶种的分散密度。随着w值的增加,晶种的分散密度增大,得到的纳米棒的分布也越稠密,反之亦然。实验结果为仅有微小出入口的密封的长微通道的功能化改性或图案化设计提供了一种新的方法。
在ZnO纳米棒阵列的基础上,在微通道的内表面上制备了Pt/ZnO, TiO2/ZnO, ZnO@ZnS等纳米棒阵列,并将这些纳米棒阵列修饰的微通道作为光催化用微反应器。以光催化降解MB溶液和4-氯苯酚溶液为例,考察了这些基于纳米棒阵列的微通道式反应器的光催化性能：
(a)基于ZnO纳米棒阵列的微通道式反应器用于光催化降解5 ppm的MB溶液,当停留时间(residence time, RT)为100s时,其对MB溶液的降解率为100%,在该停留时间下连续光催化使用180 h其对MB的降解率仍在80%以上
(b)基于分布密度可控的ZnO纳米棒花状簇的微通道式反应器用于光催化降解5 ppm的MB溶液,当停留时间大于110 s时,三根毛细管对MB的降解率都接近于100%,而在较短的停留时间(RT=25～110 s)下,毛细管M(含有中密度ZnO)较H(含有高密度ZnO)较和L(含有低密度ZnO)表现出了更强的光催化活性,表明微通道内表面上纳米棒的分布密度确实能够影响到所设计的微器件的性能。
(c)基于Pt/ZnO纳米棒阵列的微通道式反应器用于光催化降解5 ppm的MB溶液,当停留时间大于35 s时,可将MB溶液完全降解。贵金属Pt作为光生电子捕获器,有效地提高了界面电荷传递效率。
(d)基于TiO2/ZnO纳米棒阵列的微通道式反应器用于光催化降解5 ppm的MB溶液,由于TiO2和ZnO两种半导体之间的耦合作用降低了光致电子与空穴的复合,该反应器表现出了比纯的ZnO纳米棒阵列更强的光催化活性。对于不同TiO2溶胶包覆次数的TiO2/ZnO纳米棒阵列修饰的微通道的光催化活性,TiO2/ZnO-3(包覆次数为3次)表现出了最强的光催化活性。当停留时间为20s时,可将MB溶液完全降解,而且在该停留时间下,连续重复使用100 h后其对MB的降解率仍在90%以上。
(e)基于ZnO@ZnS核壳结构纳米棒阵列的微通道式反应器用于光催化降解10 ppm的MB溶液和10ppm 4-氯苯酚溶液,当停留时间为120 s时,可将MB溶液完全降解,对4-氯苯酚溶液的降解率也达到了78%。
通过光催化活性比较,基于TiO2/ZnO纳米棒阵列的微通道式反应器表现出了最强的光催化活性,且在连续重复使用时,纳米棒阵列均表现出了良好的稳定性和耐流体冲刷性。
利用连续流动的方式,通过控制Ti02溶胶的输送时间,在预制有ZnO纳米棒阵列的微通道内表面上得到了不同包覆程度的TiO2/ZnO纳米棒阵列。设计了基于TiO2/ZnO纳米棒阵列修饰的微通道的微流控器件,用于从蛋白酶解产物中选择性富集磷酸肽。以自动、连续流动的操作模式实现了蛋白酶解产物的注入、磷酸肽的富集和洗脱,且器件具有很好的选择性、灵敏性和持久性。停留时间30s富集的磷酸肽的量已足够用于MALDI-TOF MS分析。对于磷酸肽的洗脱来说,合适的停留时间为60s。鉴于该微流控器件的耐用性和连续流动的操作模式,或许会成为从大体积复杂的临床样品中高通量、选择性富集磷酸肽的一种经济有效的方法。同样,也可作为在做质谱分析前对磷酸肽进行快速和选择性富集的一种便捷手段。
利用微通道内表面上预制的ZnO纳米棒阵列作为锌源和原位模板,硫代乙酰胺则作为硫源,通过原位合成的方法在微通道内表面上得到了排列有序的ZnO@ZnS核壳结构纳米棒阵列,继续向微通道中输送巯基乙酸钠(sodium thioglycollate, ST)溶液可以得到ST-ZnO@ZnS纳米棒阵列,接着输送新鲜制备的Ag溶胶即制备出了载银Ag-ST-ZnO@ZnS纳米棒阵列。ST-ZnO@ZnS纳米棒阵列修饰的微通道对于溶液中的牛血清蛋白(bovine serum albumin, BSA)分子具有很强的吸附性,而且表现出了良好的耐用性。利用Ag-ST-ZnO@ZnS纳米棒阵列修饰微通道实现了溶液中痕量BSA分子的富集,并利用表面增强拉曼光谱(surface-enhanced Raman scattering, SERS)检测出了所富集到的BSA。基于核壳结构纳米棒阵列的微通道器件,不仅实现了从大体积生物样品中连续高通量分离蛋白,而且对于痕量蛋白的富集及检测也提出了一种简便的方法。
As one of the most advanced areas of science and technology, microfluidic technology have found many applications in various fields, ranging from life sciences to industrial chemical synthesis due to their unique advantages such as high-throughput and low-consumption. Microchannel, as an important component of microfluidic device, was just pure inner surface supplied as microspace at the early stage. However, with the development of microfluidic technology and the increasing demands for complex and improved structural functionalities of microfluidic systems for specific biological applications, modification of the inner wall of microchannels (IWMs) is necessary. Geometry modification of the microchannel is constructing specific fine micro/nano structures on the IWM. Compared with simply coating a layer of functional film on the IWMs, fabrication of micro/nanostructures perpendicular to the IWM and further grating functional groups or molecules on them can not only make the microchannel possess more functionalities, but also be considered as an important research direction promoting the microfluidic technology advancement. Various micro/nanofabrication techniques such as etching, lithography and soft lithography have been used for manufacturing micro/nanostructures to physically modify microchannel. But most of these methods are not flexible enough and are difficult to apply to a closed system such as a long microcapillary with small inlet and outlet. Moreover, the sealing process of the opened microchannel will be bound to cause damage to the formed micro/nanostructure. In this paper, a wet chemical route was used to fabricate specific micro/nanostructures on the IWM. Certain surface modifications were carried out to functionalize the constructed micro/nanostructures, and thus microchannel-based photocatalysis microreactor and micro protein enrichment device were successfully designed. Incorporating one-dimensional (1D) nanomaterials into the closed microchannel and utilizing the latest research achievements of micro/nanodevices comprising of 1D nanomaterials will open up a new way to modify and functionalize the microchannels.
ZnO nanorod arrays and distribution-tunable ZnO nanorod flowers were fabricated on the IWMs through a wet chemical route. A layer of ZnO seed film well covered on the IWM was prepared using the ethanol solutions of NaOH and Zn(AC)2·2H2O as the reactants; clusters of ZnO crystal seeds with different densities on the IWM were formed via the reverse microemulison method in which the dispersity of the micelles, the high temperature demulsification technique and the particle agglomeration all contributed to the formation. The dispersing density of crystal seeds on a substrate is of crucial importance to the selective growth and ultimate shape and morphology of crystal. So, on the IWM well covered with ZnO seed film, perpendicular growth of ZnO nanorod arrays were obtained, while on the IWM with well dispersed ZnO seed clusters, distribution density controllable ZnO nanorod flowers were fabricated. It was found that the molar ratio of water to surfactant denoted as w is an important factor which determines the dispersion of ZnO seeds and the distribution of ZnO nanorod flowers. By changing the value of w, the size of the water droplets was changed and so was the size of the particles. Also because of the different adhesion forces of the microchannel to particles with different sizes, the density of the clusters of crystal seeds was well tailored, and thus the distribution density of the final ZnO nanorod arrays was controlled. As the value of w increased, the density of the crystal seeds became bigger and the distribution of the nanorods denser. The results provide a simple, original and versatile route to generate a nano-patterned substrate in quasi closed microspace.
On the base of ZnO nanorod arrays, Pt/ZnO, TiO2/ZnO and ZnO@ZnS nanorod arrays were also fabricated on the IWM. These nanorod arrays modified microchannels were used as photocatalysis microreactors. Methylene blue (MB) and 4-chlorobenzene were chosen as model compounds to evaluate the photocatalytic activity of the microreactors.
(a) The microreactor based on ZnO nanorod arrays modified microchannel was used to photocatalyze 5 ppm MB solution. The results show that at the residence time (RT) of 100 s, the photodegradation rate of MB was over 100%and when it was repeatedly used for 180 h, the photocatalytic efficiency was still more than 80%.
(b) The microreactor based on distribution-tunable ZnO nanorod flowers modified microchannel was used to photocatalyze 5 ppm MB solution. When RT increased to more than 110 s, the photodegradation rates of MB were close to 100%for all three microreactors. However, when RT was between 25 and 110 s, microreactor M (with medium-density ZnO) showed higher photocatalytic performance than microreactor H (with high-density ZnO) and microreactor L (with medium-density ZnO), which means that the distribution density of ZnO nanorod flowers could indeed affect the performance of the as-designed microfluidic device.
(c) The microreactor based on Pt/ZnO nanorod arrays modified microchannel was used to photocatalyze 5 ppm MB solution. With RT of 35 s, the MB solution could be completely decomposed. The Pt noble metal here acts as a sink for photoinduced charge carriers, promoting interfacial charge-transfer processes.
(d) The microreactor based on TiO2/ZnO nanorod arrays modified microchannel was used to photocatalyze 5 ppm MB solution. Compared with pure ZnO nanorod arrays, the relatively more superior photocatalytic activity of the ZnO/TiO2 nanorod-modified microreactor was attributed to the combination of two semiconductors decreasing the recombination rate of photoinduced electrons and holes. Microreactor based on TiO2/ZnO-3 (TiO2 sol coating three times) showed the highest photocatalytic activity among all the microreactors based on TiO2/ZnO nanorod arrays with different TiO2 sol coating circles. For the microreactor based on TiO2/ZnO-3, RT= 20 s was sufficient to completely photodegrade MB molecules and when it was repeatedly used for 100 h, the photocatalytic efficiency of the microreactor was still more than 90%.
(e) The microreactor based on ZnO@ZnS core-shell nanorod arrays modified microchannel was used to photocatalyze 10 ppm MB solution and 10 ppm 4-chlorophenol solution. With RT of 120 s, the photodegradation rates of MB and 4-chlorophenol were 100%and 78%, respectively.
It is obvious that the microreactor based on TiO2/ZnO nanorod arrays displayed the highest photocatalytic activity among all the microreactors based on different nanorod arrays modified microchannels. Meanwhile, all the nanorod arrays showed strong washing resistance and desirable stability during the continuously recycling in photocatalysis.
A continuous-flow method was used to prepare TiO2/ZnO nanorod arrays on IWMs with different coating thicknesses. This was achieved by controlling the flow duration of a TiO2 sol in a microchannel containing preformed ZnO nanorod arrays as the supports for the immobilization of TiO2. A novel lab-on-a-chip device based on the microchannel modified with ZnO/TiO2 was designed to selectively bind and capture phosphorpeptides (PPs) from tryptic digests. This protocol allowed uninterrupted PP introduction, capture and enrichment by an automatic and continuous-flow operating mode through the microchannel. It showed great selectivity, sensitivity and durability for the enrichment of PPs from tryptic protein digests. Amounts of PPs sufficient for MALDI-MS analysis could be enriched with a RT of just 30 s. A RT of 60 s was determined to be appropriate for eluting the conjugated PPs from the CM. In view of its high durability and continuous-flow operation, this lab-on-a-chip device may achieve cost-effective, high-throughput PP enrichment from large volumes of complex clinical samples. It will also work as a convenient platform for the rapid and specific capture of PPs prior to MS analysis.
Highly-ordered ZnO@ZnS core-shell nanorod arrays were fabricated on the IWMs through an in situ conversion method with preformed ZnO nanorod arrays as the template and thioacetamide as the sulfur source. When the ZnO@ZnS nanord arrays exposed to sodium thioglycollate (ST) solution, ST-ZnO@ZnS nanorod arrays were generated on the IWC. By driving the fresh prepared Ag colloidal to the microchannel with ST-capped ZnO@ZnS nanorod arrays, Ag-loaded ST-capped ZnO@ZnS nanorod arrays on the IWC were simply obtained. The microfluidic device based on the nanorod arrays modified capillary microchannel was utilized as a novel biomolecule trapping device. Bovine serum albumin (BSA) was chosen as a model albumin to test the capture ability of the device to target protein. The microfluidic device based on ST-ZnO@ZnS nanorod arrays displayed high capture ability to BSA and high performance durability in the continuous trapping of BSA. The microfluidic device based on Ag-ST-ZnO@ZnS nanorod arrays on the IWC was also successfully applied to concentrate trace amount of BSA and the vibrational bands in the SERS results confirmed the trapped BSA. The device based on core-shell nanorod arrays on the IWC not only realized the continuous high-throughput separation of proteins from large volume complex biological matrices, but also put forward a new route to concentrate and detect trace amount of protein.
利用湿化学的方法,借助纳米技术将ZnO纳米棒阵列和分布密度可控的ZnO纳米棒花状簇集成到了石英毛细管微流控通道的内表面上。利用NaOH和Zn(AC)2·2H2O的乙醇溶液在微通道内表面上制备了一层ZnO晶种膜；利用反相微乳液法和高温去乳化作用引起的晶粒团聚,在微通道内表面上得到了分散可控的ZnO晶种。晶种在基底上的分散性对于晶体的生长及最终形貌非常重要。在完全覆盖有一层ZnO晶种膜的微通道内表面上实现了ZnO纳米棒阵列的垂直生长；在分散可控的ZnO晶种基础上实现了分布密度可控的ZnO纳米棒花状簇的生长。研究发现,水与表面活性剂的摩尔比值w是影响晶种分散和纳米棒分布密度的主要因素,通过改变w值的大小改变了水滴的大小进而改变了颗粒大小,然后借助毛细管通道内表面对于不同尺寸纳米颗粒的粘附力不同,有效地调控了晶种的分散密度。随着w值的增加,晶种的分散密度增大,得到的纳米棒的分布也越稠密,反之亦然。实验结果为仅有微小出入口的密封的长微通道的功能化改性或图案化设计提供了一种新的方法。
在ZnO纳米棒阵列的基础上,在微通道的内表面上制备了Pt/ZnO, TiO2/ZnO, ZnO@ZnS等纳米棒阵列,并将这些纳米棒阵列修饰的微通道作为光催化用微反应器。以光催化降解MB溶液和4-氯苯酚溶液为例,考察了这些基于纳米棒阵列的微通道式反应器的光催化性能：
(a)基于ZnO纳米棒阵列的微通道式反应器用于光催化降解5 ppm的MB溶液,当停留时间(residence time, RT)为100s时,其对MB溶液的降解率为100%,在该停留时间下连续光催化使用180 h其对MB的降解率仍在80%以上
(b)基于分布密度可控的ZnO纳米棒花状簇的微通道式反应器用于光催化降解5 ppm的MB溶液,当停留时间大于110 s时,三根毛细管对MB的降解率都接近于100%,而在较短的停留时间(RT=25～110 s)下,毛细管M(含有中密度ZnO)较H(含有高密度ZnO)较和L(含有低密度ZnO)表现出了更强的光催化活性,表明微通道内表面上纳米棒的分布密度确实能够影响到所设计的微器件的性能。
(c)基于Pt/ZnO纳米棒阵列的微通道式反应器用于光催化降解5 ppm的MB溶液,当停留时间大于35 s时,可将MB溶液完全降解。贵金属Pt作为光生电子捕获器,有效地提高了界面电荷传递效率。
(d)基于TiO2/ZnO纳米棒阵列的微通道式反应器用于光催化降解5 ppm的MB溶液,由于TiO2和ZnO两种半导体之间的耦合作用降低了光致电子与空穴的复合,该反应器表现出了比纯的ZnO纳米棒阵列更强的光催化活性。对于不同TiO2溶胶包覆次数的TiO2/ZnO纳米棒阵列修饰的微通道的光催化活性,TiO2/ZnO-3(包覆次数为3次)表现出了最强的光催化活性。当停留时间为20s时,可将MB溶液完全降解,而且在该停留时间下,连续重复使用100 h后其对MB的降解率仍在90%以上。
(e)基于ZnO@ZnS核壳结构纳米棒阵列的微通道式反应器用于光催化降解10 ppm的MB溶液和10ppm 4-氯苯酚溶液,当停留时间为120 s时,可将MB溶液完全降解,对4-氯苯酚溶液的降解率也达到了78%。
通过光催化活性比较,基于TiO2/ZnO纳米棒阵列的微通道式反应器表现出了最强的光催化活性,且在连续重复使用时,纳米棒阵列均表现出了良好的稳定性和耐流体冲刷性。
利用连续流动的方式,通过控制Ti02溶胶的输送时间,在预制有ZnO纳米棒阵列的微通道内表面上得到了不同包覆程度的TiO2/ZnO纳米棒阵列。设计了基于TiO2/ZnO纳米棒阵列修饰的微通道的微流控器件,用于从蛋白酶解产物中选择性富集磷酸肽。以自动、连续流动的操作模式实现了蛋白酶解产物的注入、磷酸肽的富集和洗脱,且器件具有很好的选择性、灵敏性和持久性。停留时间30s富集的磷酸肽的量已足够用于MALDI-TOF MS分析。对于磷酸肽的洗脱来说,合适的停留时间为60s。鉴于该微流控器件的耐用性和连续流动的操作模式,或许会成为从大体积复杂的临床样品中高通量、选择性富集磷酸肽的一种经济有效的方法。同样,也可作为在做质谱分析前对磷酸肽进行快速和选择性富集的一种便捷手段。
利用微通道内表面上预制的ZnO纳米棒阵列作为锌源和原位模板,硫代乙酰胺则作为硫源,通过原位合成的方法在微通道内表面上得到了排列有序的ZnO@ZnS核壳结构纳米棒阵列,继续向微通道中输送巯基乙酸钠(sodium thioglycollate, ST)溶液可以得到ST-ZnO@ZnS纳米棒阵列,接着输送新鲜制备的Ag溶胶即制备出了载银Ag-ST-ZnO@ZnS纳米棒阵列。ST-ZnO@ZnS纳米棒阵列修饰的微通道对于溶液中的牛血清蛋白(bovine serum albumin, BSA)分子具有很强的吸附性,而且表现出了良好的耐用性。利用Ag-ST-ZnO@ZnS纳米棒阵列修饰微通道实现了溶液中痕量BSA分子的富集,并利用表面增强拉曼光谱(surface-enhanced Raman scattering, SERS)检测出了所富集到的BSA。基于核壳结构纳米棒阵列的微通道器件,不仅实现了从大体积生物样品中连续高通量分离蛋白,而且对于痕量蛋白的富集及检测也提出了一种简便的方法。
As one of the most advanced areas of science and technology, microfluidic technology have found many applications in various fields, ranging from life sciences to industrial chemical synthesis due to their unique advantages such as high-throughput and low-consumption. Microchannel, as an important component of microfluidic device, was just pure inner surface supplied as microspace at the early stage. However, with the development of microfluidic technology and the increasing demands for complex and improved structural functionalities of microfluidic systems for specific biological applications, modification of the inner wall of microchannels (IWMs) is necessary. Geometry modification of the microchannel is constructing specific fine micro/nano structures on the IWM. Compared with simply coating a layer of functional film on the IWMs, fabrication of micro/nanostructures perpendicular to the IWM and further grating functional groups or molecules on them can not only make the microchannel possess more functionalities, but also be considered as an important research direction promoting the microfluidic technology advancement. Various micro/nanofabrication techniques such as etching, lithography and soft lithography have been used for manufacturing micro/nanostructures to physically modify microchannel. But most of these methods are not flexible enough and are difficult to apply to a closed system such as a long microcapillary with small inlet and outlet. Moreover, the sealing process of the opened microchannel will be bound to cause damage to the formed micro/nanostructure. In this paper, a wet chemical route was used to fabricate specific micro/nanostructures on the IWM. Certain surface modifications were carried out to functionalize the constructed micro/nanostructures, and thus microchannel-based photocatalysis microreactor and micro protein enrichment device were successfully designed. Incorporating one-dimensional (1D) nanomaterials into the closed microchannel and utilizing the latest research achievements of micro/nanodevices comprising of 1D nanomaterials will open up a new way to modify and functionalize the microchannels.
ZnO nanorod arrays and distribution-tunable ZnO nanorod flowers were fabricated on the IWMs through a wet chemical route. A layer of ZnO seed film well covered on the IWM was prepared using the ethanol solutions of NaOH and Zn(AC)2·2H2O as the reactants; clusters of ZnO crystal seeds with different densities on the IWM were formed via the reverse microemulison method in which the dispersity of the micelles, the high temperature demulsification technique and the particle agglomeration all contributed to the formation. The dispersing density of crystal seeds on a substrate is of crucial importance to the selective growth and ultimate shape and morphology of crystal. So, on the IWM well covered with ZnO seed film, perpendicular growth of ZnO nanorod arrays were obtained, while on the IWM with well dispersed ZnO seed clusters, distribution density controllable ZnO nanorod flowers were fabricated. It was found that the molar ratio of water to surfactant denoted as w is an important factor which determines the dispersion of ZnO seeds and the distribution of ZnO nanorod flowers. By changing the value of w, the size of the water droplets was changed and so was the size of the particles. Also because of the different adhesion forces of the microchannel to particles with different sizes, the density of the clusters of crystal seeds was well tailored, and thus the distribution density of the final ZnO nanorod arrays was controlled. As the value of w increased, the density of the crystal seeds became bigger and the distribution of the nanorods denser. The results provide a simple, original and versatile route to generate a nano-patterned substrate in quasi closed microspace.
On the base of ZnO nanorod arrays, Pt/ZnO, TiO2/ZnO and ZnO@ZnS nanorod arrays were also fabricated on the IWM. These nanorod arrays modified microchannels were used as photocatalysis microreactors. Methylene blue (MB) and 4-chlorobenzene were chosen as model compounds to evaluate the photocatalytic activity of the microreactors.
(a) The microreactor based on ZnO nanorod arrays modified microchannel was used to photocatalyze 5 ppm MB solution. The results show that at the residence time (RT) of 100 s, the photodegradation rate of MB was over 100%and when it was repeatedly used for 180 h, the photocatalytic efficiency was still more than 80%.
(b) The microreactor based on distribution-tunable ZnO nanorod flowers modified microchannel was used to photocatalyze 5 ppm MB solution. When RT increased to more than 110 s, the photodegradation rates of MB were close to 100%for all three microreactors. However, when RT was between 25 and 110 s, microreactor M (with medium-density ZnO) showed higher photocatalytic performance than microreactor H (with high-density ZnO) and microreactor L (with medium-density ZnO), which means that the distribution density of ZnO nanorod flowers could indeed affect the performance of the as-designed microfluidic device.
(c) The microreactor based on Pt/ZnO nanorod arrays modified microchannel was used to photocatalyze 5 ppm MB solution. With RT of 35 s, the MB solution could be completely decomposed. The Pt noble metal here acts as a sink for photoinduced charge carriers, promoting interfacial charge-transfer processes.
(d) The microreactor based on TiO2/ZnO nanorod arrays modified microchannel was used to photocatalyze 5 ppm MB solution. Compared with pure ZnO nanorod arrays, the relatively more superior photocatalytic activity of the ZnO/TiO2 nanorod-modified microreactor was attributed to the combination of two semiconductors decreasing the recombination rate of photoinduced electrons and holes. Microreactor based on TiO2/ZnO-3 (TiO2 sol coating three times) showed the highest photocatalytic activity among all the microreactors based on TiO2/ZnO nanorod arrays with different TiO2 sol coating circles. For the microreactor based on TiO2/ZnO-3, RT= 20 s was sufficient to completely photodegrade MB molecules and when it was repeatedly used for 100 h, the photocatalytic efficiency of the microreactor was still more than 90%.
(e) The microreactor based on ZnO@ZnS core-shell nanorod arrays modified microchannel was used to photocatalyze 10 ppm MB solution and 10 ppm 4-chlorophenol solution. With RT of 120 s, the photodegradation rates of MB and 4-chlorophenol were 100%and 78%, respectively.
It is obvious that the microreactor based on TiO2/ZnO nanorod arrays displayed the highest photocatalytic activity among all the microreactors based on different nanorod arrays modified microchannels. Meanwhile, all the nanorod arrays showed strong washing resistance and desirable stability during the continuously recycling in photocatalysis.
A continuous-flow method was used to prepare TiO2/ZnO nanorod arrays on IWMs with different coating thicknesses. This was achieved by controlling the flow duration of a TiO2 sol in a microchannel containing preformed ZnO nanorod arrays as the supports for the immobilization of TiO2. A novel lab-on-a-chip device based on the microchannel modified with ZnO/TiO2 was designed to selectively bind and capture phosphorpeptides (PPs) from tryptic digests. This protocol allowed uninterrupted PP introduction, capture and enrichment by an automatic and continuous-flow operating mode through the microchannel. It showed great selectivity, sensitivity and durability for the enrichment of PPs from tryptic protein digests. Amounts of PPs sufficient for MALDI-MS analysis could be enriched with a RT of just 30 s. A RT of 60 s was determined to be appropriate for eluting the conjugated PPs from the CM. In view of its high durability and continuous-flow operation, this lab-on-a-chip device may achieve cost-effective, high-throughput PP enrichment from large volumes of complex clinical samples. It will also work as a convenient platform for the rapid and specific capture of PPs prior to MS analysis.
Highly-ordered ZnO@ZnS core-shell nanorod arrays were fabricated on the IWMs through an in situ conversion method with preformed ZnO nanorod arrays as the template and thioacetamide as the sulfur source. When the ZnO@ZnS nanord arrays exposed to sodium thioglycollate (ST) solution, ST-ZnO@ZnS nanorod arrays were generated on the IWC. By driving the fresh prepared Ag colloidal to the microchannel with ST-capped ZnO@ZnS nanorod arrays, Ag-loaded ST-capped ZnO@ZnS nanorod arrays on the IWC were simply obtained. The microfluidic device based on the nanorod arrays modified capillary microchannel was utilized as a novel biomolecule trapping device. Bovine serum albumin (BSA) was chosen as a model albumin to test the capture ability of the device to target protein. The microfluidic device based on ST-ZnO@ZnS nanorod arrays displayed high capture ability to BSA and high performance durability in the continuous trapping of BSA. The microfluidic device based on Ag-ST-ZnO@ZnS nanorod arrays on the IWC was also successfully applied to concentrate trace amount of BSA and the vibrational bands in the SERS results confirmed the trapped BSA. The device based on core-shell nanorod arrays on the IWC not only realized the continuous high-throughput separation of proteins from large volume complex biological matrices, but also put forward a new route to concentrate and detect trace amount of protein.
引文
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