M. Kartel, K. Voitko, Y. Grebelna, S. Zhuravskyi, K. Ivanenko, T. Kulyk, S. Makhno, Y. Sementsov
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The available Raman spectra indicate a defective structure of GO, reduction of GO leads to greater ordering of the structure in relation to GO, nitrating and modification by amino acid - to the opposite effect, a slight deterioration of the structural state. According to the results of IR spectroscopy, also confirmed by TPD-MS, GO has a large number of functional surface groups: (OH), (C=O), (C=C), (C-O-C), (CO-O-CO), (CH). Hydrazine reduction completely hydrophobizes the surface, in the IR spectra there is only a peak at ~ 1040 cm–1, which corresponds to CO-O-CO vibrations, with significantly reduced intensity, as well as bands at 2120 and 2300 cm–1, which indicate the aromatic nature of the samples and exist in all GO derivatives. In nitrogen and sulfur-containing samples (L-GO) a new peak of ~ 1520 cm–1appears, which corresponds to N-H vibrations in amines. Sulfur-containing derivatives have valence vibrations at 600 cm–1, which most likely corresponds to S-H bonds. 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引用次数: 1
摘要
本研究的目的是发现氧化石墨烯(GO)在氮和氨基酸杂原子还原和修饰的条件下,其表面结构和状态的变化。通过水合肼(R-GO)、氮原子掺杂-尿素浸渍和热处理(N-GO)还原氧化石墨烯,并通过亲核加成(L-GO)对氧化石墨烯表面进行含硫氨基酸- l -半胱氨酸修饰。采用拉曼散射、红外光谱、tpd质谱、动态光散射等分析方法对样品进行了表征。可用的拉曼光谱表明氧化石墨烯的结构有缺陷,氧化石墨烯的还原导致与氧化石墨烯相关的结构更有序,氨基酸的硝化和修饰-相反的效果,结构状态轻微恶化。红外光谱结果和TPD-MS证实,氧化石墨烯具有大量的表面官能团:(OH)、(C=O)、(C=C)、(C-O-C)、(CO-O-CO)、(CH)。在红外光谱中,仅在~ 1040 cm-1处有一个峰,对应于CO-O-CO振动,强度明显减弱;在2120和2300 cm-1处有两个谱带,表明样品具有芳香性,所有GO衍生物都存在。在含氮和含硫样品(L-GO)中,出现了~ 1520 cm - 1的新峰,对应于胺中的N-H振动。含硫衍生物的价振动在600 cm-1,这很可能对应于S-H键。因此,氧化石墨烯的修饰会导致其结构和表面化学发生重大变化,从而影响所得样品捕获自由基的能力。以往的实证研究表明,该性质的增加顺序为L-GO > GO > N-GO > R-GO。
Changes in the structure and properties of graphene oxide surfaces during reduction and modification
The aim of the current study was to find changes in the structure and state of the surface of graphene oxide (GO) under the conditions of its reduction and modification by hetero atoms of nitrogen and amino acids. Reduction of GO was performed with hydrazine hydrate (R-GO), doping with nitrogen atoms - urea impregnation and subsequent heat treatment (N-GO), and the surface of GO was modified with sulfur-containing amino acid – L-cysteine by nucleophilic addition (L-GO). The samples obtained were characterized by analytical methods, such as Raman scattering, IR spectroscopy, TPD-mass-spectrometry, dynamic light scattering spectroscopy. The available Raman spectra indicate a defective structure of GO, reduction of GO leads to greater ordering of the structure in relation to GO, nitrating and modification by amino acid - to the opposite effect, a slight deterioration of the structural state. According to the results of IR spectroscopy, also confirmed by TPD-MS, GO has a large number of functional surface groups: (OH), (C=O), (C=C), (C-O-C), (CO-O-CO), (CH). Hydrazine reduction completely hydrophobizes the surface, in the IR spectra there is only a peak at ~ 1040 cm–1, which corresponds to CO-O-CO vibrations, with significantly reduced intensity, as well as bands at 2120 and 2300 cm–1, which indicate the aromatic nature of the samples and exist in all GO derivatives. In nitrogen and sulfur-containing samples (L-GO) a new peak of ~ 1520 cm–1appears, which corresponds to N-H vibrations in amines. Sulfur-containing derivatives have valence vibrations at 600 cm–1, which most likely corresponds to S-H bonds. Thus, modification of GO leads to a significant change in its structure and surface chemistry, which in turn affects the capability of the obtained samples to capture free radicals. Previous empirical studies have shown that this property increases in the series L-GO > GO > N-GO > R-GO.