一维纳米杂化材料的光电传感性质及在环境检测中的研究
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摘要
单壁碳纳米管(SWCNTs)自其被发现以来,就以其独特的结构和性质吸引人们广泛的关注。在其众多性质中,首要的应该是它们的电学性质,它们通常是作为电学材料来使用。高的电荷淌度和优良的弹道输运特性将使它们能在未来的电器设备中成为替代硅的最佳材料。此外,单壁碳纳米管(SWCNTs)融合到传统的场效应晶体管(FET)的结构中,还能充分发挥场效应管的特性。就其应用而言,由于其特有的准一维电子结构和超高的比表面积,使得用它们为材料制成的传感器有着传统传感器无法比拟的优越性。
另外,具有独特光学性质的一维金纳米颗粒(Gold Nanorods)也是人们关注的热点,它们在有机-无机化合物,光电子学,生物材料和生物医药等方面都有着潜在的应用。金纳米颗粒有一个重要的性质,那就是当经过一定频率的入射光照射后,其表面的电子会产生相应的振荡,这种现象称为表面等离子共振(SPR)。而表面等离子共振(SPR)的强度和波长对周围环境反应非常敏感,通过表面增强Raman (SERS)的测量,可以利用这一特性进行传感性研究。
无论是单壁碳纳米管(SWCNTs)还是金纳米颗粒(Gold Nanorods)都是很好的传感材料,它们将会在未来的传感器研究和发展中起到十分重要的作用。本论文主要采用合成的一些敏感材料对碳纳米管(SWCNTs)和金纳米棒(Gold Nanorods)进行了化学修饰,并研究了它们的传感性。主要内容如下：
一、首次合成了两个含六氟异丙醇基团(HFIP)的化合物,对六氟异丙醇苯胺(HFIPA)和N-4-六氟异丙醇苯基-1-芘丁酰胺(HFIPP),并分别用它们修饰单壁碳纳米管(SWCNTs),得到两个碳管杂化材料SWCNT-HFIPP及SWCNT-HFIPPH。考虑到六氟异丙醇基团(HFIP)与神经毒剂沙林之间能形成强烈的氢键作用,所合成的两个复合材料分别被制作成化学微传感器并对沙林的模拟物甲基磷酸二甲酯(DMMP)进行了检测,测试结果表明它们对DMMP的响应表现出很高的灵敏性和选择性,可以预测这两种材料在未来爆炸物及其它化学战剂的检测中能发挥潜在的作用。
二、首次合成了一个环糊精衍生物：单-6-脱氧-6-对氨基苯氨基-β-环糊精(PCD),并通过重氮化反应将PCD修饰到单壁碳纳米管(SWCNTs)上,得到一个新的单壁碳纳米管杂化材料(SWCNT-PCD)。基于环糊精有很好的分子识别性,该杂化材料被制成了化学电阻型传感器,并用它对自然界中的持久有机污染物(POPs)进行了检测,结果展现出优良的灵敏性和选择性。研究还表明传感器电导的变化率随PCD和不同POPs分子之间的结合常数的增大而增大,可以预测该传感器在环境检测中有着潜在的应用。
三、合成了不同长径比的一维金纳米棒(Gold Nanorods),并用单-6-巯基-p-环糊精对它们进行化学修饰,得到金纳米棒的复合材料,其特殊的结构提高了对农残分子的捕捉力,第一次使用这种材料的表面增强Raman效应(SERS)对农残甲基对硫膦进行了检测。研究表明长径比为二的金纳米棒能表现出更好的SERS效应。由于环糊精的空腔能与甲基对硫膦形成有效地结合体,通过SERS光谱中的指纹峰强度的识别,农残能被检测到皮摩尔级。相对于其它传统的农残检测方法,这种使用无Raman标签的杂化一维金纳米棒材料为SERS基底,在农残检测中能表现出优良的灵敏性和选择性。
As new carbon materials, Single-Walled Carbon Nanotubes (SWCNTs) have attracted great interests recently due to their unique chemical and physical properties. Particularly, applications of SWCNTs based on electrical properties are being widely investigated, which lead to their considerations as replacements for Si in future generation devices. Considered that SWCNTs can be well compatible with conventional field-effect transistor (FET) architectures, SWCNT-FET with quasi-one-dimensional electronic structures and very high surface-to-volume ratios can be expected as excellent electronic nanodevices compared to tranditional sensors.
On the other hand, the unique optical properties of gold nanostructures also attract a great deal of attention due to their potential applications in organic-inorganic composites, photonics, biomaterials, and biomedicine. It should be noted that intensity and wavelength of surface plasmon resonance (SPR) of one-dimesional gold nanoparticles (Gold Nanorods), viz., coherent oscillations of the metal electrons in resonance with light of a certain frequency, are highly sensitive to the surrounding environment, which can be utilized for surface enhanced Raman scattering (SERS) sensing purposes. Strong enhancement of the electromagnetic field owing to the excitation of the surface plasmons at the surface of particles have been extensively studied for sensing applications.
In summary, sensing hybridized materials of SWCNTs and Gold Nanorods (GNRs) can be expected as excellent candidates to manufacture future generations of chemical sensors. In this dissertation, hybridized SWCNTs or GNRs have been prepared and employed to fabricate sensing devices, which display excellent sensitivity and selectivity. The main conclusions are summarized as follows:
(1) Two novel compounds, N-4-Hexafluoroisopropanolphenyl-l-pyrenebutyramide (HFIPP) and p-hexafluoroisopropanol aniline (HFIPA) have been prepared for the first time. After functionalized with SWCNTs, two new hybridized materials SWCNT-HFIPP and SWCNT-HFIPPH have been obtained. Considered that strong hydrogen-bonding can be formed between hexafluoroisopropanol groups and dimethyl methylphosphonate (DMMP) (simulant of nerve agent sarin), two hybridized material sensing devices have been fabricated and utilized to detect DMMP. Excellent sensitivity and selectivity of the hybridized devices suggest that they have great capability of detecting explosives and chemical warfare agents.
(2) Novel SWCNT-PCD hybrids have been successfully synthesized through in situ diazonium reaction between mono-6-deoxy-6-(p-aminophenylamino)-β-cyclodextrin (PCD) and SWCNTs for the first time. The cyclodextrin (CD) groups bind to the SWCNT surfaces through covalent interactions. Based on the sensing materials, fabricated chemical sensors of SWCNT-PCD hybrids have been utilized to detect Persistent Organic Pollutants (POPs), which exhibit excellent sensitivity and selectivity due to the concept of molecular recognition. The equilibrium constant values for the complexation of the PCD with the different POPs correlate with the magnitudes of the conductance change ratios of the SWCNT-PCD devices after binding of these POPs molecules, which can be suggested as potential applications in environmental monitor.
(3) The as-prepared GNRs with different aspect ratios have been decorated with mono-6-thio-β-cyclodextrin so as to efficiently capture and detect methyl parathion insecticide via surface enhanced Raman scattering (SERS) technique for the first time. Detailed comparison among different aspect ratios of the GNRs suggests that the GNRs with aspect ratio 2 can be provided as excellent SERS active substrate for detecting the insecticide in the present study. Due to efficient formation of host-guest between hybridized cavity and methyl parathion, identification of the insecticide can be observed at picomolar level according to the fingerprint Raman peaks. Excellent sensitivity and selectivity for detection of the insecticide using the hybridized GNRs without Raman label indicate that it is a simple and ultrasensitive approach for detecting insecticides in contrast with some other traditional detection approaches.
另外,具有独特光学性质的一维金纳米颗粒(Gold Nanorods)也是人们关注的热点,它们在有机-无机化合物,光电子学,生物材料和生物医药等方面都有着潜在的应用。金纳米颗粒有一个重要的性质,那就是当经过一定频率的入射光照射后,其表面的电子会产生相应的振荡,这种现象称为表面等离子共振(SPR)。而表面等离子共振(SPR)的强度和波长对周围环境反应非常敏感,通过表面增强Raman (SERS)的测量,可以利用这一特性进行传感性研究。
无论是单壁碳纳米管(SWCNTs)还是金纳米颗粒(Gold Nanorods)都是很好的传感材料,它们将会在未来的传感器研究和发展中起到十分重要的作用。本论文主要采用合成的一些敏感材料对碳纳米管(SWCNTs)和金纳米棒(Gold Nanorods)进行了化学修饰,并研究了它们的传感性。主要内容如下：
一、首次合成了两个含六氟异丙醇基团(HFIP)的化合物,对六氟异丙醇苯胺(HFIPA)和N-4-六氟异丙醇苯基-1-芘丁酰胺(HFIPP),并分别用它们修饰单壁碳纳米管(SWCNTs),得到两个碳管杂化材料SWCNT-HFIPP及SWCNT-HFIPPH。考虑到六氟异丙醇基团(HFIP)与神经毒剂沙林之间能形成强烈的氢键作用,所合成的两个复合材料分别被制作成化学微传感器并对沙林的模拟物甲基磷酸二甲酯(DMMP)进行了检测,测试结果表明它们对DMMP的响应表现出很高的灵敏性和选择性,可以预测这两种材料在未来爆炸物及其它化学战剂的检测中能发挥潜在的作用。
二、首次合成了一个环糊精衍生物：单-6-脱氧-6-对氨基苯氨基-β-环糊精(PCD),并通过重氮化反应将PCD修饰到单壁碳纳米管(SWCNTs)上,得到一个新的单壁碳纳米管杂化材料(SWCNT-PCD)。基于环糊精有很好的分子识别性,该杂化材料被制成了化学电阻型传感器,并用它对自然界中的持久有机污染物(POPs)进行了检测,结果展现出优良的灵敏性和选择性。研究还表明传感器电导的变化率随PCD和不同POPs分子之间的结合常数的增大而增大,可以预测该传感器在环境检测中有着潜在的应用。
三、合成了不同长径比的一维金纳米棒(Gold Nanorods),并用单-6-巯基-p-环糊精对它们进行化学修饰,得到金纳米棒的复合材料,其特殊的结构提高了对农残分子的捕捉力,第一次使用这种材料的表面增强Raman效应(SERS)对农残甲基对硫膦进行了检测。研究表明长径比为二的金纳米棒能表现出更好的SERS效应。由于环糊精的空腔能与甲基对硫膦形成有效地结合体,通过SERS光谱中的指纹峰强度的识别,农残能被检测到皮摩尔级。相对于其它传统的农残检测方法,这种使用无Raman标签的杂化一维金纳米棒材料为SERS基底,在农残检测中能表现出优良的灵敏性和选择性。
As new carbon materials, Single-Walled Carbon Nanotubes (SWCNTs) have attracted great interests recently due to their unique chemical and physical properties. Particularly, applications of SWCNTs based on electrical properties are being widely investigated, which lead to their considerations as replacements for Si in future generation devices. Considered that SWCNTs can be well compatible with conventional field-effect transistor (FET) architectures, SWCNT-FET with quasi-one-dimensional electronic structures and very high surface-to-volume ratios can be expected as excellent electronic nanodevices compared to tranditional sensors.
On the other hand, the unique optical properties of gold nanostructures also attract a great deal of attention due to their potential applications in organic-inorganic composites, photonics, biomaterials, and biomedicine. It should be noted that intensity and wavelength of surface plasmon resonance (SPR) of one-dimesional gold nanoparticles (Gold Nanorods), viz., coherent oscillations of the metal electrons in resonance with light of a certain frequency, are highly sensitive to the surrounding environment, which can be utilized for surface enhanced Raman scattering (SERS) sensing purposes. Strong enhancement of the electromagnetic field owing to the excitation of the surface plasmons at the surface of particles have been extensively studied for sensing applications.
In summary, sensing hybridized materials of SWCNTs and Gold Nanorods (GNRs) can be expected as excellent candidates to manufacture future generations of chemical sensors. In this dissertation, hybridized SWCNTs or GNRs have been prepared and employed to fabricate sensing devices, which display excellent sensitivity and selectivity. The main conclusions are summarized as follows:
(1) Two novel compounds, N-4-Hexafluoroisopropanolphenyl-l-pyrenebutyramide (HFIPP) and p-hexafluoroisopropanol aniline (HFIPA) have been prepared for the first time. After functionalized with SWCNTs, two new hybridized materials SWCNT-HFIPP and SWCNT-HFIPPH have been obtained. Considered that strong hydrogen-bonding can be formed between hexafluoroisopropanol groups and dimethyl methylphosphonate (DMMP) (simulant of nerve agent sarin), two hybridized material sensing devices have been fabricated and utilized to detect DMMP. Excellent sensitivity and selectivity of the hybridized devices suggest that they have great capability of detecting explosives and chemical warfare agents.
(2) Novel SWCNT-PCD hybrids have been successfully synthesized through in situ diazonium reaction between mono-6-deoxy-6-(p-aminophenylamino)-β-cyclodextrin (PCD) and SWCNTs for the first time. The cyclodextrin (CD) groups bind to the SWCNT surfaces through covalent interactions. Based on the sensing materials, fabricated chemical sensors of SWCNT-PCD hybrids have been utilized to detect Persistent Organic Pollutants (POPs), which exhibit excellent sensitivity and selectivity due to the concept of molecular recognition. The equilibrium constant values for the complexation of the PCD with the different POPs correlate with the magnitudes of the conductance change ratios of the SWCNT-PCD devices after binding of these POPs molecules, which can be suggested as potential applications in environmental monitor.
(3) The as-prepared GNRs with different aspect ratios have been decorated with mono-6-thio-β-cyclodextrin so as to efficiently capture and detect methyl parathion insecticide via surface enhanced Raman scattering (SERS) technique for the first time. Detailed comparison among different aspect ratios of the GNRs suggests that the GNRs with aspect ratio 2 can be provided as excellent SERS active substrate for detecting the insecticide in the present study. Due to efficient formation of host-guest between hybridized cavity and methyl parathion, identification of the insecticide can be observed at picomolar level according to the fingerprint Raman peaks. Excellent sensitivity and selectivity for detection of the insecticide using the hybridized GNRs without Raman label indicate that it is a simple and ultrasensitive approach for detecting insecticides in contrast with some other traditional detection approaches.
引文
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