Construction of Three-dimensional Graphene/oxygen-enriched Vacancy Fe2O3 Composites to Realize Ultra-high Energy Density of Supercapacitors

doi:10.6023/A24120372

Acta Chimica Sinica ›› 2025, Vol. 83 ›› Issue (3): 256-265.DOI: 10.6023/A24120372 Previous Articles Next Articles

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三维石墨烯/富含氧空位Fe₂O₃复合材料的构建实现超级电容器超高能量密度

孙伟^a^,^b^,^c, 辛国祥^a^,^b^,^c^,^*(), 刘飞^a^,^b^,^c, 鞠藤^a^,^b^,^c, 程宇通^a^,^b^,^c, 宋金玲^a^,^b^,^c, 包金小^a^,^b^,^c^,^*(), 布林朝克^a^,^b^,^c

a 内蒙古科技大学材料科学与工程学院包头 014010
b 内蒙古自治区先进陶瓷材料与器件重点实验室包头 014010
c 轻稀土资源绿色提取与高效利用教育部重点实验室(内蒙古科技大学) 包头 014010

投稿日期:2024-12-17 发布日期:2025-02-17
基金资助:
国家自然科学基金(22462023); 内蒙古自然科学基金(2020ZD17); 内蒙古自然科学基金(2021MS05011); 内蒙古自治区直属高校基本科研业务费项目(2023QNJS018); 内蒙古自治区直属高校基本科研业务费项目(2024YXXS038); 内蒙古自治区高校创新科研团队项目(NMGIRT2215)

Construction of Three-dimensional Graphene/oxygen-enriched Vacancy Fe₂O₃ Composites to Realize Ultra-high Energy Density of Supercapacitors

Wei Sun^a^,^b^,^c, Guoxiang Xin^a^,^b^,^c(), Fei Liu^a^,^b^,^c, Teng Ju^a^,^b^,^c, Yutong Cheng^a^,^b^,^c, Jinling Song^a^,^b^,^c, Jinxiao Bao^a^,^b^,^c(), Chaoke Bulin^a^,^b^,^c

a School of Materials Science and Engineering, Inner Mongolia University of Science and Technology, Baotou 014010, China
b Inner Mongolia Key Laboratory of Advanced Ceramic Material and Devices, Baotou 014010, China
c Key Laboratory of Green Extraction & Efficient Utilization of Light Rare-Earth Resources (Inner Mongolia University of Science and Technology), Ministry of Education, Baotou 014010, China

Received:2024-12-17 Published:2025-02-17
Contact: ^*E-mail: xinguoxiang@imust.edu.cn; baojinxiao@imust.cn
Supported by:
National Natural Science Foundation of China(22462023); Natural Science Foundation of Inner Mongolia(2020ZD17); Natural Science Foundation of Inner Mongolia(2021MS05011); basic research funds for universities directly under Inner Mongolia Autonomous Region(2023QNJS018); basic research funds for universities directly under Inner Mongolia Autonomous Region(2024YXXS038); Program for Innovative Research Team in Universities of Inner Mongolia Autonomous Region, China(NMGIRT2215)

Iron trioxide (Fe₂O₃) possesses the high theoretical capacitance, and the improvement of its deficiency of low electric conductivity can be performed by the oxygen vacancy engineering strategy. The combination of Fe₂O₃ with oxygen vacancies (OV-Fe₂O₃) and graphene with high conductivity is expected to obtain high energy density. In this study, the construction of three-dimensional reduced graphene oxide/OV-Fe₂O₃ (3D rGO/OV-Fe₂O₃) composite is completed through the complexation-reduction method under the hydrothermal reduction condition. The typical synthesis procedure is described as follows. First, 0.6 g of Fe(NO₃)₃•9H₂O was dissolved into 15 mL of deionized water, then added 0.27 g of polyethylene glycol-2000, stirred for 10 min, and then added 12.5 mL of GO solution (8 mg•mL⁻¹). After stirring the mixed solution for 20 min and ultrasonic vibration for 20 min, 2 mL of hydrazine hydrate was added into the mixing solution, and then stirred for 20 min and ultrasonically vibrated for 20 min again. Subsequently, the prepared mixed solution was transferred into a reactor for hydrothermal reaction. The reaction temperature was retained 180 ℃ for 12 h. After the hydrothermal reaction, the obtained sample was washed with deionized water and finally placed in a freeze dryer for 24 h to obtain the 3D rGO/OV-Fe₂O₃ composite. The nano-scaled OV-Fe₂O₃ shows the irregular geometric polyhedrons by the observation of morphology, which was uniformly distributed on the surface of 3D rGO or within the three-dimensional pores. The presence of oxygen vacancies is indicated via the X-ray diffraction pattern, electron paramagnetic resonance spectroscopy, and X-ray photoelectron spectroscopy. Electrochemical tests manifest that the specific capacitance of 3D rGO/OV-Fe₂O₃ is as high as 928.3 F•g⁻¹. The assembled asymmetric supercapacitor 3D rGO/OV-Fe₂O₃||3D rGO delivers an ultra-high energy density up to 95.1 Wh•kg⁻¹. The capacitance retention rate is 94% after 20000 cycles. The ideal supercapacitive performance of 3D rGO/OV-Fe₂O₃||3D rGO is attributed to the improvement of the electrical conductivity of Fe₂O₃ due to the creation of oxygen vacancies in its lattice structure and the providing of three-dimensional conducting channels owing to the construction of 3D rGO. As supercapacitor electrode material, the 3D rGO/OV-Fe₂O₃ has a broad prospect.

Key words: hydrothermal reduction, oxygen vacancy, iron trioxide, reduced graphene oxide, high energy density, asymmetric supercapacitor

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Wei Sun, Guoxiang Xin, Fei Liu, Teng Ju, Yutong Cheng, Jinling Song, Jinxiao Bao, Chaoke Bulin. Construction of Three-dimensional Graphene/oxygen-enriched Vacancy Fe₂O₃ Composites to Realize Ultra-high Energy Density of Supercapacitors[J]. Acta Chimica Sinica, 2025, 83(3): 256-265.

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Fig. & Tab. 8

Figure 1. Schematic for the hydrothermal synthesis of 3D rGO/ OV-Fe2O3

Figure 2. (a) XRD patterns, (b) Raman spectra and (c) TGA curves of GO, 3D rGO, OV-Fe2O3 and 3D rGO/OV-Fe2O3; (d) EPR spectra of OV-Fe2O3 and 3D rGO/OV-Fe2O3

Figure 3. SEM images of (a) 3D rGO and (b~d) 3D rGO/OV-Fe2O3

Figure 4. (a~c) Low magnification TEM images, (d, e) HRTEM images, (f) selected area electron diffraction (SAED) images of 3D rGO/OV-Fe2O3, (g~i) elemental mappings of Fe, C and O elements for (b)

Figure 5. XPS spectra and fitting peaks of 3D rGO/OV-Fe2O3: (a) full spectrum, (b) C1s, (c) O 1s, (d) Fe 2p

Figure 6. (a) N2 absorption/desorption curves and (b) pore size distribution of 3D rGO/OV-Fe2O3 and 3D rGO/Fe2O3

Figure 7. Electrochemical properties in the three-electrode system: (a) CV profiles of 3D rGO, OV-Fe2O3, 3D rGO/Fe2O3 and 3D rGO/OV-Fe2O3 at a scan rate of 100 mV?s?1, (b) CV curves of 3D rGO/OV-Fe2O3 at different scan rates, (c) Plot of log(peak current) vs. log(scan rate), (d) Comparison of the total and capacitive contributions of 3D rGO/OV-Fe2O3 by CV at 100 mV?s?1, (e) The ratios of the diffusion and surface-capacitance contributions at different scan rates of 3D rGO/OV-Fe2O3, (f) GCD curves of 3D rGO, OV-Fe2O3, 3D rGO/Fe2O3 and 3D rGO/OV-Fe2O3 under a current density of 1 A?g?1, (g) GCD curves of 3D rGO/OV-Fe2O3 at different current densities, (h) Nyquist plots of 3D rGO, OV-Fe2O3, 3D rGO/Fe2O3 and 3D rGO/OV-Fe2O3. The top-right inset shows the equivalent circuit diagram, and the bottom-right inset shows their magnified plots at the high frequency region, (i) Capacitance retention plots of 3D rGO/Fe2O3 and 3D rGO/OV-Fe2O3 for 20000 cycles at a current density of 2 A?g?1

Figure 8. Electrochemical properties of 3D rGO/OV-Fe2O3||3D rGO asymmetric supercapacitor: (a) assembled schematic illustration, (b) CV curves of 3D rGO/OV-Fe2O3 and 3D rGO at a scan rate of 100 mV?s?1, (c) CV curves measured at different potential windows of 1.2~1.5 V at a scan rate of 100 mV?s?1, (d) CV curves at different scan rates, (e) GCD curves at different current densities, (f) Nyquist plot, (g) Ragone plots of 3D rGO/OV-Fe2O3||3D rGO compared to recent reports, (h) capacitance retention and coulombic efficiency at a current density of 2 A?g?1 for 20000 cycles, and the photographs in the inset shows three 3D rGO/OV-Fe2O3||3D rGOs connected in series can light up a blue LED light

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三维石墨烯/富含氧空位Fe₂O₃复合材料的构建实现超级电容器超高能量密度

Construction of Three-dimensional Graphene/oxygen-enriched Vacancy Fe₂O₃ Composites to Realize Ultra-high Energy Density of Supercapacitors

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三维石墨烯/富含氧空位Fe2O3复合材料的构建实现超级电容器超高能量密度