Effects of different mass ratios of tetrabutyl titanate on the microstructure and properties of GO?TiO2 composite materials
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摘要: 以氧化石墨烯和鈦酸四丁酯為原料，采用一步水熱法制備氧化石墨烯/二氧化鈦（GO?TiO2）復合材料，研究不同鈦酸四丁酯含量對GO?TiO2復合材料組織和性能的影響規律。通過掃描電鏡（SEM）、X射線衍射（XRD）、紅外光譜（IR）、拉曼光譜（RS）、紫外?可見分光光度計（UV?vis）、熱重分析儀（TGA）等對復合材料的微觀形貌、物相組成、結構、吸光性和熱穩定性進行表征。研究結果表明，隨著鈦酸四丁酯含量的增加，有利于GO?TiO2復合材料的均勻分散，提高了GO?TiO2復合材料的吸光性和熱穩定性，但鈦酸四丁酯含量過高會使GO?TiO2復合材料分散性、吸光性和熱穩定性下降。當氧化石墨烯質量為320 mg、鈦酸四丁酯含量為100 mL時，反應生成的復合材料表面TiO2分散均勻，缺陷少，D峰與G峰的峰強比（ID/IG）值為0.91，氧化石墨烯和二氧化鈦復合程度高，復合材料中的TiO2吸收邊緣紅移至可見光范圍內，并且在440~800 nm可見光范圍內的吸收峰明顯增強，防腐防污能力增強，復合材料在800 ℃熱穩定性相比于氧化石墨烯提高了84.89%。Abstract: Graphene oxide/titanium dioxide (GO–TiO2) composites were prepared via a one-step hydrothermal synthesis method using graphene oxide and tetrabutyl titanate as raw materials. The effects of different mass ratios of tetrabutyl titanate on the microstructure and properties of the GO–TiO2 composites were studied. The microscopic morphology of these composites was observed through a scanning electron microscope, and the phase composition and structure were analyzed using X-ray diffraction, infrared spectroscopy, and Raman spectroscopy. The light absorption performance and thermal stability of the composites were analyzed via ultraviolet–visible spectroscopy and a thermal gravimetric analyzer. As the content of tetrabutyl titanate increases, the TiO2 generation increases; material surface area climbs up and then declines; surface defects decline and then climb up; absorption peak in the visible light range strengthens and then weakens; and degree of recombination climbs up and then weakens. When the content of tetrabutyl titanate exceeded 100 mL, the dispersibility of TiO2 in the GO–TiO2 composites became poor, thereby reducing the light absorption performance and thermal stability of the composites. When the GO was 320 mg and tetrabutyl titanate was 100 mL in the precursor solution, the obtained composite material exhibited superior surface properties, optical properties, and thermal stability. TiO2 was uniformly dispersed on the surface of the composite material. The composite material exhibited a high absorption intensity of visible light, high recombination, few surface defects, and an ID/IG ratio of 0.91. Characteristic peaks at 1573 and 1428 cm?1 were the strongest. The absorption edge of TiO2 in the composite was bathochromic shifted to the visible light range, and the absorption peak was significantly enhanced in the visible light range of 440–800 nm. The composite material exhibited good anticorrosion and antifouling abilities. The thermal stability of the composite was 84.89% higher than that of GO at 800°C. These composites have great prospects for development in the fields of anticorrosion and antifouling.
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圖 2 不同鈦酸四丁酯含量的GO?TiO2的SEM和EDX圖. SEM:(a) GO; (b)1#;(c) 2#; (d)3#; (e)4#; (f) 5#; EDX : (g) 面掃; (h) 元素原子比
Figure 2. SEM and EDX images of GO–TiO2 composites with different mass ratios of tetrabuty titanate: SEM of (a) GO; (b) 1#; (c) 2#; (d) 3#; (e) 4#; (f) 5#; and EDS of (g) mapping; (h) atomic ratio of element
圖 3 不同鈦酸四丁酯含量的GO?TiO2的XRD圖
Figure 3. XRD images of GO–TiO2 composites with different mass ratios of tetrabutyl titanate
圖 4 氧化石墨烯和不同鈦酸四丁酯含量的GO?TiO2的紅外光譜
Figure 4. FT–IR spectra of GO and GO–TiO2 composites with different mass ratios of tetrabutyl titanate
圖 5 不同鈦酸四丁酯含量的GO?TiO2的拉曼光譜圖. (a) 波數為50~800 cm?1; (b) 波數為800~4000 cm?1
Figure 5. Raman spectra images of GO–TiO2 composites with different mass ratios of tetrabutyl titanate: (a) wavenumber of 50–800 cm?1; (b) wavenumber of 800–4000 cm?1
圖 6 不同鈦酸四丁酯含量的GO?TiO2的紫外可見吸收光譜
Figure 6. UV?vis spectra of GO–TiO2 composites with different mass ratios of tetrabutyl titanate
圖 7 不同鈦酸四丁酯含量的GO?TiO2的TG圖
Figure 7. TG images of GO–TiO2 composites with different mass ratios of tetrabutyl titanate
表 1 不同鈦酸四丁酯的含量
Table 1. Different mass ratios of tetrabutyl titanate
Number Graphene oxide /mg Tetrabutyl titanate/mL 1# 320 40 2# 320 60 3# 320 80 4# 320 100 5# 320 120 
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表 2 不同鈦酸四丁酯含量的GO?TiO2的ID/IG值
Table 2. ID/IG of GO–TiO2 composites with different mass ratios of tetrabutyl titanate
Number ID/IG GO 1.181 1# 1.069 2# 1.049 3# 1.002 4# 0.91 5# 0.948
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