摘要
随着纳米光电子学研究的深入,特殊功能的纳米复合光电材料已逐渐成为研究热点。由于具有大的共轭体系,碳纳米管(CNTs)在高速低耗的光电子器件、光伏电池等方面具有应用前景。通过多种功能化和分析方法研究不同结构碳纳米管的光电性质已经成为实现其应用价值的重要途径。本文以单壁CNTs (SWNT)和少壁CNTs (FWNT)为研究对象,研究其制备和室温纯化,功能化及其各项光电性质,为其进一步在纳米光电器件领域的应用提供依据。
以液相室温氧化法对气相沉积法(CVD)法制备的FWNT粗产物进行纯化,透射电镜(TEM)显示粗产物在H_2O_2中缓慢氧化1w后可得到产率为10%高纯FWNT。拉曼光谱和热失重分析表明H_2O_2可以选择性地去除产物中的碳杂质,但不会破坏FWNT的管壁和化学结构。选择CNTs和Na2PdCl4的质量比为1:4,得到金属钯纳米粒子(平均粒径为7.3 nm)表面修饰的SWNT和FWNT。与纯CNTs相比,SWNT/Pd NPs和FWNT/Pd NPs薄膜的导电率分别提高了近5倍和2倍。分离结果显示钯纳米粒子更倾向于选择性地附着在金属态SWNT表面。通过N-取代共价键合方法制备3,4,9,10-N,N’-甲基芘-苝酰亚胺(PDI-PY),利用芘和CNTs之间的π-π共轭吸附作用,合成了高效宽谱吸收的PDI-PY/CNTs复合体。通过PDI-PY与SWNT的选择性非共价功能化,能有效地分离金属态和半导体态SWNT。
通过HNO_3质子化获得具有一系列高导电FWNT透明薄膜,以此为电极制备结构为FWNT/P3HT:PCBM/Al的有机光伏电池。结果显示最佳光伏器件(FWNT薄膜T=70%, Rs=86Ω/□)的光电转换效率为0.61%,与以ITO为电极的相同电池的转换效率(0.68%)相近。所得到的三维网状FWNT薄膜易于导电聚合物的交叉渗入,有利于光伏性能的提高。通过共价键合法制备三种具有不同电子推拉结构的偶氮苯生色团-CNTs复合体(SWNT-AZO-NO_2、FWNT-chain-AZO、MWNT-AZO-NH_2)。偶氮苯与CNTs共轭体系的相互作用导致SWNT-AZO-NO_2和MWNT-AZO-NH_2中的偶氮苯生色团的吸收峰发生了蓝移和红移,在紫外光诱导下,与SWNT-AZO-NO_2和MWNT-AZO-NH_2相比,碳纳米管和偶氮苯之间的长烷基链导致FWNT-chain-AZO呈现出快速敏感的光响应特性,偏振光初步结果显示偶氮苯基团的光致取向作用使MWNT-AZO-NH_2薄膜呈现各向异性,碳纳米管在与入射偏振光平行的方向上有序程度提高并发生定向排列,这一结果为设计具有快速敏感的光响应的偶氮苯-CNTs各向异性薄膜提供了重要的实验基础。
The development of nano-optoelectronic strongly relies on the discovery and exploration of new functional opto-electrical nanocomposites as a vital component of active layer. Since the discovery, carbon nanotubes (CNTs) were widely regarded as an ideal candidate to the building block of a series of high-response and low-cost opto-electronics such as optical switch, photodetecotor and photovoltaic devices due to favorable electron transport along with one-dimension tube-structure arising from highπ-conjugated system. Therefore, the researches on the opto-electrical properties of functional CNTs are fundamentally significant to actualize the applicable potential. In this thesis, we systematically focused on a profitable route from materials to application, and that is the synthesis, purification, functionalization and photoconversion devices based on single-walled carbon nanotubes (SWNT) and few-walled carbon nanotubes (FWNT). Results illustrated the relationship between opto-electical properties and devices, which are experimentally and theoretically important to potential applications.
Highly purified FWNT was processed by room temperature purification in 30 wt % H2O_2 for 1 week with the yield up to 10 %. Raman spectra and TGA characterization indicated that H_2O_2 purification selectively oxidized carbonaceous nano-particles without the damage of the structure of FWNT. A new versatile and simple way of SWNT and FWNT decorated by Palladium nanoparticles (Pd NPs) was presented. Optimal decoration was achieved with a large amount of sphere-shape Pd NPs on the sidewall when weight ratio of CNTs and Na_2PdCl_4 is 1:4. Compared with original CNTs film, the conductivity of SWNT/Pd-NPs and FWNT/Pd-NPs film were enhanced up to 2 fold and 5 fold. Raman spectra showed that Pd NPs tended to be deposited on metallic SWNT. Organic conjugated molecule of N,N’1’-methyl- pyrene-3,4,9,10-perylene diimide (PDI-PY) was synthesized by covalent N-substitution. PDI-PY/SWNT and PDI-PY/FWNT nanocomposites with high and board absorption spectra were prepared byπ-electron stacking. Raman spectra indicated that metallic and semiconducting enriched SWNT were selectively separated due to different solubility in organic solvents after the functionalization.
Organic photovoltaic devices (OPD) using high conductive transparent few-walled carbon nanotubes (FWNT) electrode was fabricated. Maximum efficiency of OPD up to 0.61 % with the structure of FWNT (transparency, T=70 %, sheet resistance, Rs = 86Ω/□)/ poly(3-hexylthiophene) : [6-6]phenyl-C61-butyric acid methyl ester /Al demonstrated a promising alternative of ITO (0.68 %) with almost identical operation. The performance improvement resulted from the optimal balance between sheet resistance and transparency with three-dimensional network interface between nanotubes and polymers. A series of photoresponsive azobenzene chromophore-CNTs nanocomposites with different push-pull electronic groups (SWNT-AZO-NO_2,FWNT-chain-AZO,MWNT-AZO-NH_2) were synthesized via covalent amide reaction. The electronic interaction between azobenzene moiety and CNTs resulted in the red- and blue-shifts in absorption spectra of SWNT-AZO-NO_2 and MWNT-AZO-NH_2. Compared with SWNT-AZO-NO_2 and MWNT-AZO-NH_2, FWNT-chain-AZO with the alkyl chain between azobenzene and sidewall displayed a faster photoresponse due to weakenedπ-electron stacking and enough free-space for the photoisomerizion azobenzene chromophore. Polarization results preliminarily indicated the anisopic MWNT-AZO-NH_2 film due to the photo-induced alignment of nanotubes in the direction parallel to the electric field vector of polarized light by the photo-orientation of azobenzene chromphore. Results offer a great promise to fast photosensitive AZO-CNTs anisotropic film.
引文
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