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

doi:10.6023/A24120372

化学学报 ›› 2025, Vol. 83 ›› Issue (3): 256-265.DOI: 10.6023/A24120372 上一篇下一篇

研究论文

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)

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摘要/Abstract

氧化铁(Fe₂O₃)具有高的理论电容, 氧空位工程策略可改善其导电率低的不足, 将含氧空位的Fe₂O₃ (OV-Fe₂O₃)与高导电率的石墨烯复合, 有望获得高能量密度. 本研究在水热还原条件下采用络合-还原法构建三维还原氧化石墨烯/OV-Fe₂O₃ (3D rGO/OV-Fe₂O₃)复合材料. 通过形貌观察, 纳米级OV-Fe₂O₃呈不规则几何多面体在3D rGO表面或三维孔隙内均匀分布. X射线衍射谱、电子顺磁共振谱和X射线光电子能谱表明Fe₂O₃中氧空位的存在. 电化学测试表明, 3D rGO/OV-Fe₂O₃比电容高达928.3 F•g⁻¹. 组装的非对称超级电容器3D rGO/OV-Fe₂O₃||3D rGO的能量密度高达95.1 Wh•kg⁻¹, 20000次循环后的电容保持率达94%. 3D rGO/OV-Fe₂O₃||3D rGO理想的超电容性能归因于Fe₂O₃晶格结构中氧空位的产生改善了Fe₂O₃的导电率, 同时3D rGO的构建也为OV-Fe₂O₃提供了三维导电通道. 3D rGO/OV-Fe₂O₃作为超级电容器电极材料具有广阔前景.

关键词: 水热还原, 氧空位, 氧化铁, 还原氧化石墨烯, 高能量密度, 非对称超级电容器

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

引用此文

孙伟, 辛国祥, 刘飞, 鞠藤, 程宇通, 宋金玲, 包金小, 布林朝克. 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[J]. 化学学报, 2025, 83(3): 256-265.

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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图/表 8

图1. 3D rGO/OV-Fe2O3的水热合成示意图

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

图2. GO, 3D rGO, OV-Fe2O3和3D rGO/OV-Fe2O3的(a) XRD谱, (b) Raman谱和(c) TGA曲线; (d) OV-Fe2O3和3D rGO/OV-Fe2O3的EPR谱

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

图3. (a) 3D rGO和(b~d) 3D rGO/OV-Fe2O3的SEM图

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

图4. 3D rGO/OV-Fe2O3的(a~c)低倍TEM图, (d, e) HRTEM图, (f)选择区域电子衍射(SAED)图, (g~i)图b对应的Fe, C和O元素分布图

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)

图5. 3D rGO/OV-Fe2O3的XPS谱: (a)总谱, (b) C 1s, (c) O 1s, (d) Fe 2p的分峰图

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

图6. 3D rGO/OV-Fe2O3和3D rGO/Fe2O3的(a) N2吸/脱附曲线和(b)孔径分布图

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

图7. 三电极体系下电化学性能: (a)扫描速率为100 mV?s?1时3D rGO、OV-Fe2O3、3D rGO/Fe2O3和3D rGO/OV-Fe2O3的CV曲线, (b) 3D rGO/OV-Fe2O3在不同扫描速率下的CV曲线, (c)扫描速率与峰值电流的对数函数图, (d)在100 mV?s?1扫速下总贡献和电容贡献的比较, (e) 3D rGO/OV-Fe2O3在不同扫描速率下的扩散和表面电容贡献比, (f)电流密度为1 A?g?1时3D rGO、OV-Fe2O3、3D rGO/Fe2O3和3D rGO/OV-Fe2O3的GCD曲线, (g)不同电流密度下3D rGO/OV-Fe2O3的GCD曲线, (h) 3D rGO、OV-Fe2O3、3D rGO/Fe2O3和3D rGO/OV-Fe2O3的Nyquist图. 右上角的插图为等效电路图, 右下角的插图为高频区域的放大图, (i) 3D rGO/Fe2O3和3D rGO/OV-Fe2O3在电流密度为2 A?g?1的条件下20000次循环的电容保持率图

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

图8. 3D rGO/OV-Fe2O3||3D rGO非对称超级电容器的电化学性质: (a)组装示意图, (b) 3D rGO/OV-Fe2O3和3D rGO在100 mV?s?1下CV曲线, (c)在1.2~1.5 V不同电位窗下测得CV曲线, 扫描速率为100 mV?s?1, (d)不同扫描速率下的CV曲线, (e)不同电流密度下的GCD曲线, (f) Nyquist图, (g) 3D rGO/OV-Fe2O3||3D rGO的Ragone图与最近报道的比较, (h)循环20000次的电容保持率和库伦效率, 电流密度为2 A?g?1, 插图显示三个3D rGO/OV-Fe2O3||3D rGO串联可点亮蓝色LED灯

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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