无机碳、硒纳米颗粒催化鲁米诺化学发光反应的机理研究
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摘要
以化学反应为基础的化学发光分析法具有灵敏度高、线性范围宽、仪器设备简单、分析速度快等诸多优点,已成为重要的分析方法之一。其中鲁米诺发光体系因具有较高的发光量子产率和较好的水溶性,是目前研究及应用最为广泛的一类化学发光试剂。近年来,随着纳米技术的发展,鲁米诺化学发光已从传统的分子或离子范围拓展到纳米科学领域。然而,纳米颗粒参与的鲁米诺发光体系依然有限,同时许多有关鲁米诺化学发光的报道都只进行了机理的推测或依据少量的实验事实提出可能的反应机理,但研究反应机理的实验手段实际上相对较少,并没有真正获取反应中间体或产物的详细信息。因此,研究新的纳米材料参与的化学发光体系及发光机理已成为化学发光领域的重要课题。基于此,本论文主要围绕碳纳米材料和铜硫族化物纳米颗粒催化鲁米诺的化学发光机理开展了一系列研究。主要内容如下：
1.发现氧化石墨烯(Graphene oxide, GO)做为催化剂可以提高鲁米诺-过氧化氢体系的化学发光强度,并且其催化过程是通过单线态氧(1O2)的中间产物完成的,这和文献上报道的其它纳米材料催化通过羟自由基(OH.)和超氧阴离子自由基(O2-)的中间产物截然不同。研究表明,在弱碱性介质中,GO能够增强鲁米诺-过氧化氢体系的化学发光强度,与单壁碳纳米管(Single-walled carbon nanotubes, SWCNTs)、多壁碳纳米管(Multiwalled carbon nanotubes, MWCNTs)及碳纳米颗粒(Carbon nanoparticles, CNPs)相比,GO具有更强的催化能力,这主要归因于它的高比表面积(理论值为2630m2/g)。同时,GO的催化能力比还原型氧化石墨烯(Red uced graphene oxide, RGO)也强,这主要是因为GO表面的含氧官能基团在催化过程中发挥了重要的作用。以GO催化鲁米诺-过氧化氢的化学发光体系为例,考察了溶液pH值、反应试剂浓度(鲁米诺、过氧化氢及GO溶液)等参数对体系发光的影响,并借助化学发光光谱、紫外-可见吸收光谱、电子顺磁共振(Electron paramagnetic resonance, EPR)光谱、各类自由基捕获实验等手段研究该化学发光增强的机理。结果表明,与以往传统催化剂催化鲁米诺发光机制不同的是,该发光过程为典型的1O2诱导的发光机理,其原因是具有大共轭结构的GO在催化过氧化氢分解时首先生成OH·和O2·-,自由基间(如OH·和O2·-)的再聚合和重组反应导致在其表面生成大量的1O2；最后,1O2和鲁米诺反应生成激发态的3-氨基邻苯二甲酸根离子(3-APA*,鲁米诺的氧化产物)并产生位于440nm的化学发光。因此,在上述发光体系中,1O2和鲁米诺间的反应是占主导地位的。我们的实验结果大大地丰富了传统鲁米诺的发光机理,相信其在生化分析等领域将具有更广泛的应用。
2.发现十六烷基三甲基溴化铵包被的碳点(Cetyltrimethyl ammonium bromide-carbon nanodots, CTAB-CDs)在强碱性介质中可显著地提高鲁米诺-过氧化氢体系的化学发光强度。更重要的是,该提高过程是通过1O2的中间产物实现的,这和大多数的文献报道是不同的。CDs因其良好的性能被研究者们广泛关注,它的优良催化活性主要是其表面特殊结构与反应物之间相互作用的结果。我们以CTAB为钝化剂,采用富勒烯(C60)水热法合成CTAB-CDs,研究发现其在强碱性介质中能够明显增强鲁米诺-过氧化氢的化学发光20倍,其催化活性明显优于GO。基于CTAB-CDs加入前后鲁米诺-过氧化氢体系的化学发光光谱、动力学光谱、紫外-可见吸收光谱、EPR光谱和透射电子显微镜图(Transmission electron microscopy, TEM)的变化,及不同的自由基捕获剂对该体系化学发光强度的影响,提出了CTAB-CDs增敏鲁米诺发光的机理。与GO相同,CTAB-CDs催化鲁米诺发光的过程仍为典型的1O2诱导的发光机理,其原因可能为：水热法合成CDs的过程中,C60大的共轭结构并未被完全破坏,这样合成的CDs仍会保留C60的部分共轭结构。而共轭结构的存在不但会加速过氧化氢分解生成OH·和O2·-,而且还能进一步促进两者相互反应生成1O2。这项工作不仅有利于我们更好地理解碳纳米材料的表面性质和化学反应活性,而且丰富了强碱性介质条件下传统的鲁米诺发光机理,为化学发光分析法注入了新的活力。
3.半导体铜硫属化物纳米颗粒-硒化铜(Cu2-xSe)可以增强鲁米诺-过氧化氢体系的化学发光,诱导发光增强的关键中间产物经证明是OH·和O2·-。实验发现,在强碱性介质中,Cu2-xSe对鲁米诺-过氧化氢体系的发光信号具有极大的增强作用(至少增强500倍),推测这与它特殊的结构,尤其是其中的铜元素或铜缺陷紧密相关。通过自由基抑制剂的抑制作用、化学发光光谱、紫外-可见吸收光谱、扫描电子显微镜图(Scanning electron microscope, SEM)、EPR光谱等手段,证实了OH.和02-在发光过程中起着关键作用,但这两种自由基并没有在Cu2-xSe表面进一步反应生成’02。所以,在上述体系中,OH-和02-是诱导Cu2-xSe催化鲁米诺发光增强的关键自由基,这和常规的纳米催化过程是一致的。
4.纳米颗粒的结构,尤其是大的共轭结构的存在对102诱导鲁米诺-过氧化氢体系的发光机制有很大的影响。研究了强碱性介质条件下金胶(AuNPs)、银胶(AgNPs)及GO/Cu2-xSe复合物三种纳米颗粒的催化过程。结果表明,AuNPs、 AgNPs的表面并没有1O2生成,而GO/Cu2-xSe的表面则生成了大量的1O2。在我们选择的6种纳米材料中,按照表面是否有大的共轭结构可分为两大类。有共轭结构的包括GO、CTAB-CDs和GO/Cu2-xSe,在催化鲁米诺发光的过程中,它们不但能加速电子转移和催化过氧化氢分解成氧自由基,而且还能使上述氧自由基发生进一步的重组反应,那么其催化过程就为典型的1O2诱导的发光机理；另一大类没有共轭结构的纳米材料包括AuNPs、AgNPs和Cu2-xSe,它们在催化鲁米诺发光的过程中,仅能加速电子转移和催化过氧化氢分解生成OH.和O2-,大的共轭结构的缺失导致上述两种自由基不能进一步反应生成1O2。所以,纳米颗粒上大的共轭结构的存在至关重要,这直接决定了诱导体系发光的关键氧自由基。
以上实验结果表明,将纳米颗粒作为催化剂应用于鲁米诺化学发光分析中,极大地拓展了化学发光的理论和应用研究范畴。对于催化机理而言,具有大的共轭结构的纳米粒子具有加速自由基产生并使自由基重组的作用,即它们除了加速电子转移和催化过氧化氢分解生成OH.和O2-,在其表面还可以发生自由基间(如OH.和O2-)的重组反应从而生成大量的102。上述结果对深入认识鲁米诺的化学发光机理、纳米颗粒独特的结构和功能性质,以及进一步拓展其在分析化学等相关领域中的应用,无疑具有重要的意义。
As a common luminescence phenomenon, chemiluminescence (CL) is based on a chemical reaction, and has been an attractive topic of intensive researches in various fields because of its high sensitivity, wide linear dynamic range, simple instrumentation, fast analysis, and low background. Among many well-established CL reagents, luminol is the most frequently used due to the relatively high luminescent quantum yield and good water solubility. Recently, with the development of nanotechnology, the CL of luminol has been extended to nanoparticles (NPs) systems in addition to traditional molecular or ionic systems. Higher sensitivity and stability can be achieved by using the NPs owing to their large surface area and special structures. However, the NPs-participated CL of luminol is still limited. On the other hand, many reported literatures on luminol CL only contained the assumption on the mechanism or proposed the possible luminescent processes on the basis of a few experimental data. The reaction mechanism was rarely studied by experimental methods, so we can hardly get the detailed information of the reaction intermediates. Therefore, it is an important issue to develop a new NPs-involved CL and further investigate its chemiluminescent mechanism. In this contribution, we attempt to establish the carbon-and metal chalcogenide nanomaterials-catalyzed luminol CL systems and carry out a series of studies on their enhancement mechanism. The main contains are listed as follows:
1. Graphene oxide (GO) was found to enhance the CL of luminol-H2O2system mainly through the intermediate of1O2, which was greatly different from the traditional catalyst in such CL system that occurred in a strongly basic medium through the intermediates such as superoxide anion radical (O2-) and hydroxyl radical (OH-). In this work, GO could catalyze the luminol-H2O2CL in a weakly alkaline medium, and the GO-enhanced CL is markedly stronger than that of the other carbon materials including CNPs, MWCNTs, or SWCNTs, which is attributed to the high specific surface area of GO (calculated value,2630m2/g). Moreover, the effect of GO on luminol CL seems to be much stronger than that of RGO, owing to the oxygen-related groups of GO which are indeed a reactive part and crucial for luminol CL. Furthermore, taking GO-catalyzed luminol-H2O2CL as an example, we used CL spectral, UV-visible absorption spectral, and EPR spectral measurements and the effects of various free radical scavengers on the GO-enhanced luminol CL to identify the possible CL enhancement mechanism. The results showed that the enhancement took place mainly through the intermediate of1O2. It is well known that GO has a large conjugated structure, which can accelerate electron-transfer processes and the generation of radical species, as well as improve their stability. That is, the addition of GO into luminol system could not only catalyze the decomposition of H2O2to produce OH· and O2·-, but also facilitate the recombination reaction between them to form a high yield of1O2on the surface of GO. Then, the resulted1O2then reacted with luminol, producing an endoperoxide which decomposed to the excited state3-aminophthalate anions (3-APA*), and giving rise to light emission with the maximum wavelength at440nm. So the CL reaction between1O2and luminol to produce the3-APA*must be dominant in the present CL syetem. This work enriches greatly luminol CL mechanism, which would be of great potential applications in nanomaterial-based analytical chemistry.
2. Cetyltrimethyl ammonium bromide passivated carbon nanodots (CTAB-CDs) can be used as excellent catalysts to dramatically enhance the CL intensity of luminol-H2O2system in NaOH medium. More importantly, this CL enhancement takes place mainly through the intermediate of1O2, which follows a different mechanism from traditional reports. CDs attract growing attention in many fields because of their excellent catalytic activity, which may result from the interactions between their unique surface structure and the reagents. In this work, we prepared a new kind of CTAB-CDs through the hydrothermal method, using fullerene (C60) as the raw material in the presence of CTAB. The CTAB-CDs can enhance the CL intensity of luminol-H2O2system in NaOH medium up to20times, and show a better CL catalytic ability than that of GO reported in our previous work. The CL spectra, UV-vis spectra, EPR spectra, and transmission electron microscopy (TEM) images before and after the CL reaction, as well as the effects of various free radical scavengers on the CL intensity were all conducted to identify the possible CL enhancement mechanism. Similar to GO, the enhanced CL by CTAB-CDs was still attributed to the1O2-induced luminescent mechanism. During the process of hydrothermal synthesis of CTAB-CDs, the conjugate structure of Cf,o has not been completely destroyed, and thus the as-formed CTAB-CDs may keep partly the conjugate structure of C60. The existence of the conjugated structure of CTAB-CDs could decompose H2O2effectively into OH-and O2-, which then participated in the radical recombination reaction to form plenty of O2on the surfaces of CTAB-CDs. Therefore, the enhanced CL of the CDs-based luminol system in NaOH solution was primarily caused by1O2, rather than other reported oxygen radicals. The present study is beneficial not only for gaining a better understanding of the1O2-induced luminol CL mechanism in a strongly alkaline medium, but also displaying the unique surface property and chemical reactivity of CDs.
3. The semiconductor chalcogenide nanomaterial, copper selenide (Cu2-xSe), was found to catalyze the chemiluminescent reaction between luminol and H2O2, and the key intermediates induced luminescence enhancement were the OH-and O2-. The experimental results showed that Cu2-xSe NPs could enhance the CL signal of luminol-H2O2system more than500folds in alkaline medium. The strong catalytic ability of this kind of NPs is probably attribulted to the critical roles of copper element or copper defects. Based on the CL spectra, UV-vis spectra, EPR spectra, and scanning electron microscope (SEM) images before and after the CL reaction, as well as the effects of various free radical scavengers on the CL intensity, we considered that OH-and O2-played an important role in luminol CL enhancement. In other words, these two kinds of free radicals did not further react with each other to form O2on the surface of Cu2-xSe NPs. Therefore, OH-and O2-, instead of1O2, were the key species for the emission processes, which was identical with the common nanocatalytical systems.
4. The structure of NPs, especially the large conjugate structure, has a great influence on the1O2-induced luminescence mechanism. We also studied the catalytic activity of AuNPs, AgNPs and GO/Cu2-xSe in strong alkaline conditions. The results indicated that1O2did not generate on the surfaces of both AuNPs and AgNPs. On the contrary, abundant1O2was observed on the surface of GO/Cu2-xSe. We supposed that the NPs used as catalysts could accelerate the electron transfer and decomposition of H2O2to produce oxygen-related intermediates, and may play an important role in making them react with each other to form1O2as well. As for the NPs including GO, CTAB-CDs, and GO/Cu2-xSe, their catalytical processes can be the typical1O2-induced luminescence mechanism because of the presence of the conjugated structure. However, for the Cu2-xSe, AuNPs, and AgNPs, the generation of1O2from OH·and O2-could not occur due to the absence of the large conjugated structure, and the role of these NPs was only to accelerate the electron transfer and the decomposion of H2O2. Therefore, the large conjugated structure on the surface of NPs is a critical factor, which directly determines the key radicals in the process of luminol CL.
The above experimental results indicate that, the NPs are introduced into the luminol CL system as the catalysts, which can remarkably expand the theory and applications of CL. As for the mechanism, the existence of large conjugated structure of the NPs can accelerate the generation of free radicals, and further make them recombination. That is, the NPs with the large conjugated structure can catalyze the electron transfer and the decomposition of H2O2to form OH·and O2-,and then they react with each other to form abundant1O2. In summary, the research results described above would be important for deeply understanding the CL mechanism of luminol and the properties of NPs, and helpful to expand their applications in a variety of fields.
1.发现氧化石墨烯(Graphene oxide, GO)做为催化剂可以提高鲁米诺-过氧化氢体系的化学发光强度,并且其催化过程是通过单线态氧(1O2)的中间产物完成的,这和文献上报道的其它纳米材料催化通过羟自由基(OH.)和超氧阴离子自由基(O2-)的中间产物截然不同。研究表明,在弱碱性介质中,GO能够增强鲁米诺-过氧化氢体系的化学发光强度,与单壁碳纳米管(Single-walled carbon nanotubes, SWCNTs)、多壁碳纳米管(Multiwalled carbon nanotubes, MWCNTs)及碳纳米颗粒(Carbon nanoparticles, CNPs)相比,GO具有更强的催化能力,这主要归因于它的高比表面积(理论值为2630m2/g)。同时,GO的催化能力比还原型氧化石墨烯(Red uced graphene oxide, RGO)也强,这主要是因为GO表面的含氧官能基团在催化过程中发挥了重要的作用。以GO催化鲁米诺-过氧化氢的化学发光体系为例,考察了溶液pH值、反应试剂浓度(鲁米诺、过氧化氢及GO溶液)等参数对体系发光的影响,并借助化学发光光谱、紫外-可见吸收光谱、电子顺磁共振(Electron paramagnetic resonance, EPR)光谱、各类自由基捕获实验等手段研究该化学发光增强的机理。结果表明,与以往传统催化剂催化鲁米诺发光机制不同的是,该发光过程为典型的1O2诱导的发光机理,其原因是具有大共轭结构的GO在催化过氧化氢分解时首先生成OH·和O2·-,自由基间(如OH·和O2·-)的再聚合和重组反应导致在其表面生成大量的1O2；最后,1O2和鲁米诺反应生成激发态的3-氨基邻苯二甲酸根离子(3-APA*,鲁米诺的氧化产物)并产生位于440nm的化学发光。因此,在上述发光体系中,1O2和鲁米诺间的反应是占主导地位的。我们的实验结果大大地丰富了传统鲁米诺的发光机理,相信其在生化分析等领域将具有更广泛的应用。
2.发现十六烷基三甲基溴化铵包被的碳点(Cetyltrimethyl ammonium bromide-carbon nanodots, CTAB-CDs)在强碱性介质中可显著地提高鲁米诺-过氧化氢体系的化学发光强度。更重要的是,该提高过程是通过1O2的中间产物实现的,这和大多数的文献报道是不同的。CDs因其良好的性能被研究者们广泛关注,它的优良催化活性主要是其表面特殊结构与反应物之间相互作用的结果。我们以CTAB为钝化剂,采用富勒烯(C60)水热法合成CTAB-CDs,研究发现其在强碱性介质中能够明显增强鲁米诺-过氧化氢的化学发光20倍,其催化活性明显优于GO。基于CTAB-CDs加入前后鲁米诺-过氧化氢体系的化学发光光谱、动力学光谱、紫外-可见吸收光谱、EPR光谱和透射电子显微镜图(Transmission electron microscopy, TEM)的变化,及不同的自由基捕获剂对该体系化学发光强度的影响,提出了CTAB-CDs增敏鲁米诺发光的机理。与GO相同,CTAB-CDs催化鲁米诺发光的过程仍为典型的1O2诱导的发光机理,其原因可能为：水热法合成CDs的过程中,C60大的共轭结构并未被完全破坏,这样合成的CDs仍会保留C60的部分共轭结构。而共轭结构的存在不但会加速过氧化氢分解生成OH·和O2·-,而且还能进一步促进两者相互反应生成1O2。这项工作不仅有利于我们更好地理解碳纳米材料的表面性质和化学反应活性,而且丰富了强碱性介质条件下传统的鲁米诺发光机理,为化学发光分析法注入了新的活力。
3.半导体铜硫属化物纳米颗粒-硒化铜(Cu2-xSe)可以增强鲁米诺-过氧化氢体系的化学发光,诱导发光增强的关键中间产物经证明是OH·和O2·-。实验发现,在强碱性介质中,Cu2-xSe对鲁米诺-过氧化氢体系的发光信号具有极大的增强作用(至少增强500倍),推测这与它特殊的结构,尤其是其中的铜元素或铜缺陷紧密相关。通过自由基抑制剂的抑制作用、化学发光光谱、紫外-可见吸收光谱、扫描电子显微镜图(Scanning electron microscope, SEM)、EPR光谱等手段,证实了OH.和02-在发光过程中起着关键作用,但这两种自由基并没有在Cu2-xSe表面进一步反应生成’02。所以,在上述体系中,OH-和02-是诱导Cu2-xSe催化鲁米诺发光增强的关键自由基,这和常规的纳米催化过程是一致的。
4.纳米颗粒的结构,尤其是大的共轭结构的存在对102诱导鲁米诺-过氧化氢体系的发光机制有很大的影响。研究了强碱性介质条件下金胶(AuNPs)、银胶(AgNPs)及GO/Cu2-xSe复合物三种纳米颗粒的催化过程。结果表明,AuNPs、 AgNPs的表面并没有1O2生成,而GO/Cu2-xSe的表面则生成了大量的1O2。在我们选择的6种纳米材料中,按照表面是否有大的共轭结构可分为两大类。有共轭结构的包括GO、CTAB-CDs和GO/Cu2-xSe,在催化鲁米诺发光的过程中,它们不但能加速电子转移和催化过氧化氢分解成氧自由基,而且还能使上述氧自由基发生进一步的重组反应,那么其催化过程就为典型的1O2诱导的发光机理；另一大类没有共轭结构的纳米材料包括AuNPs、AgNPs和Cu2-xSe,它们在催化鲁米诺发光的过程中,仅能加速电子转移和催化过氧化氢分解生成OH.和O2-,大的共轭结构的缺失导致上述两种自由基不能进一步反应生成1O2。所以,纳米颗粒上大的共轭结构的存在至关重要,这直接决定了诱导体系发光的关键氧自由基。
以上实验结果表明,将纳米颗粒作为催化剂应用于鲁米诺化学发光分析中,极大地拓展了化学发光的理论和应用研究范畴。对于催化机理而言,具有大的共轭结构的纳米粒子具有加速自由基产生并使自由基重组的作用,即它们除了加速电子转移和催化过氧化氢分解生成OH.和O2-,在其表面还可以发生自由基间(如OH.和O2-)的重组反应从而生成大量的102。上述结果对深入认识鲁米诺的化学发光机理、纳米颗粒独特的结构和功能性质,以及进一步拓展其在分析化学等相关领域中的应用,无疑具有重要的意义。
As a common luminescence phenomenon, chemiluminescence (CL) is based on a chemical reaction, and has been an attractive topic of intensive researches in various fields because of its high sensitivity, wide linear dynamic range, simple instrumentation, fast analysis, and low background. Among many well-established CL reagents, luminol is the most frequently used due to the relatively high luminescent quantum yield and good water solubility. Recently, with the development of nanotechnology, the CL of luminol has been extended to nanoparticles (NPs) systems in addition to traditional molecular or ionic systems. Higher sensitivity and stability can be achieved by using the NPs owing to their large surface area and special structures. However, the NPs-participated CL of luminol is still limited. On the other hand, many reported literatures on luminol CL only contained the assumption on the mechanism or proposed the possible luminescent processes on the basis of a few experimental data. The reaction mechanism was rarely studied by experimental methods, so we can hardly get the detailed information of the reaction intermediates. Therefore, it is an important issue to develop a new NPs-involved CL and further investigate its chemiluminescent mechanism. In this contribution, we attempt to establish the carbon-and metal chalcogenide nanomaterials-catalyzed luminol CL systems and carry out a series of studies on their enhancement mechanism. The main contains are listed as follows:
1. Graphene oxide (GO) was found to enhance the CL of luminol-H2O2system mainly through the intermediate of1O2, which was greatly different from the traditional catalyst in such CL system that occurred in a strongly basic medium through the intermediates such as superoxide anion radical (O2-) and hydroxyl radical (OH-). In this work, GO could catalyze the luminol-H2O2CL in a weakly alkaline medium, and the GO-enhanced CL is markedly stronger than that of the other carbon materials including CNPs, MWCNTs, or SWCNTs, which is attributed to the high specific surface area of GO (calculated value,2630m2/g). Moreover, the effect of GO on luminol CL seems to be much stronger than that of RGO, owing to the oxygen-related groups of GO which are indeed a reactive part and crucial for luminol CL. Furthermore, taking GO-catalyzed luminol-H2O2CL as an example, we used CL spectral, UV-visible absorption spectral, and EPR spectral measurements and the effects of various free radical scavengers on the GO-enhanced luminol CL to identify the possible CL enhancement mechanism. The results showed that the enhancement took place mainly through the intermediate of1O2. It is well known that GO has a large conjugated structure, which can accelerate electron-transfer processes and the generation of radical species, as well as improve their stability. That is, the addition of GO into luminol system could not only catalyze the decomposition of H2O2to produce OH· and O2·-, but also facilitate the recombination reaction between them to form a high yield of1O2on the surface of GO. Then, the resulted1O2then reacted with luminol, producing an endoperoxide which decomposed to the excited state3-aminophthalate anions (3-APA*), and giving rise to light emission with the maximum wavelength at440nm. So the CL reaction between1O2and luminol to produce the3-APA*must be dominant in the present CL syetem. This work enriches greatly luminol CL mechanism, which would be of great potential applications in nanomaterial-based analytical chemistry.
2. Cetyltrimethyl ammonium bromide passivated carbon nanodots (CTAB-CDs) can be used as excellent catalysts to dramatically enhance the CL intensity of luminol-H2O2system in NaOH medium. More importantly, this CL enhancement takes place mainly through the intermediate of1O2, which follows a different mechanism from traditional reports. CDs attract growing attention in many fields because of their excellent catalytic activity, which may result from the interactions between their unique surface structure and the reagents. In this work, we prepared a new kind of CTAB-CDs through the hydrothermal method, using fullerene (C60) as the raw material in the presence of CTAB. The CTAB-CDs can enhance the CL intensity of luminol-H2O2system in NaOH medium up to20times, and show a better CL catalytic ability than that of GO reported in our previous work. The CL spectra, UV-vis spectra, EPR spectra, and transmission electron microscopy (TEM) images before and after the CL reaction, as well as the effects of various free radical scavengers on the CL intensity were all conducted to identify the possible CL enhancement mechanism. Similar to GO, the enhanced CL by CTAB-CDs was still attributed to the1O2-induced luminescent mechanism. During the process of hydrothermal synthesis of CTAB-CDs, the conjugate structure of Cf,o has not been completely destroyed, and thus the as-formed CTAB-CDs may keep partly the conjugate structure of C60. The existence of the conjugated structure of CTAB-CDs could decompose H2O2effectively into OH-and O2-, which then participated in the radical recombination reaction to form plenty of O2on the surfaces of CTAB-CDs. Therefore, the enhanced CL of the CDs-based luminol system in NaOH solution was primarily caused by1O2, rather than other reported oxygen radicals. The present study is beneficial not only for gaining a better understanding of the1O2-induced luminol CL mechanism in a strongly alkaline medium, but also displaying the unique surface property and chemical reactivity of CDs.
3. The semiconductor chalcogenide nanomaterial, copper selenide (Cu2-xSe), was found to catalyze the chemiluminescent reaction between luminol and H2O2, and the key intermediates induced luminescence enhancement were the OH-and O2-. The experimental results showed that Cu2-xSe NPs could enhance the CL signal of luminol-H2O2system more than500folds in alkaline medium. The strong catalytic ability of this kind of NPs is probably attribulted to the critical roles of copper element or copper defects. Based on the CL spectra, UV-vis spectra, EPR spectra, and scanning electron microscope (SEM) images before and after the CL reaction, as well as the effects of various free radical scavengers on the CL intensity, we considered that OH-and O2-played an important role in luminol CL enhancement. In other words, these two kinds of free radicals did not further react with each other to form O2on the surface of Cu2-xSe NPs. Therefore, OH-and O2-, instead of1O2, were the key species for the emission processes, which was identical with the common nanocatalytical systems.
4. The structure of NPs, especially the large conjugate structure, has a great influence on the1O2-induced luminescence mechanism. We also studied the catalytic activity of AuNPs, AgNPs and GO/Cu2-xSe in strong alkaline conditions. The results indicated that1O2did not generate on the surfaces of both AuNPs and AgNPs. On the contrary, abundant1O2was observed on the surface of GO/Cu2-xSe. We supposed that the NPs used as catalysts could accelerate the electron transfer and decomposition of H2O2to produce oxygen-related intermediates, and may play an important role in making them react with each other to form1O2as well. As for the NPs including GO, CTAB-CDs, and GO/Cu2-xSe, their catalytical processes can be the typical1O2-induced luminescence mechanism because of the presence of the conjugated structure. However, for the Cu2-xSe, AuNPs, and AgNPs, the generation of1O2from OH·and O2-could not occur due to the absence of the large conjugated structure, and the role of these NPs was only to accelerate the electron transfer and the decomposion of H2O2. Therefore, the large conjugated structure on the surface of NPs is a critical factor, which directly determines the key radicals in the process of luminol CL.
The above experimental results indicate that, the NPs are introduced into the luminol CL system as the catalysts, which can remarkably expand the theory and applications of CL. As for the mechanism, the existence of large conjugated structure of the NPs can accelerate the generation of free radicals, and further make them recombination. That is, the NPs with the large conjugated structure can catalyze the electron transfer and the decomposition of H2O2to form OH·and O2-,and then they react with each other to form abundant1O2. In summary, the research results described above would be important for deeply understanding the CL mechanism of luminol and the properties of NPs, and helpful to expand their applications in a variety of fields.
引文
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