Composite electrode material and preparation method and application thereof

[0029] Example 1

[0030] (1) Preparation of N-GQDS: 0.42 g of citric acid and 0.36 g of urea at 30 ml H 2 The ultrasonic dispersion of O. The mixed solution was transferred to 50 ml of the inner liner in the stainless steel autoclave of polytetrafluoroethylene, and heated at 180 ° C for 5 hours; the product was centrifuged at 12000 rpm for 20 minutes, take the supernatant at 80 ° C Dry N-Gqd powder, configured to concentrate 1 mg · ml -1 N-GQDS aqueous solution.

[0031] (2) Preparation of Ni-Mof / NF: 1.2G Ni (NO) 3 )2 • 6h 2 O and 2.6 g 2-methylimidazole (2-Mi) were dissolved in 80 mL distilled water, pour 2-Mi aqueous solution into NI (NO 3 ) 2 • 6h 2 O Aqueous solution is stirred for 10 minutes to obtain a mixed solution, take a piece of cut into 1 × 3 cm 2 Foam nickel is placed in a mixed solution for 2 hours, was washed several times with water and ethanol, and dried at 60 ° C for 5 hours to obtain Ni-Mof / NF;

[0032] (3) Preparation of NiGA-LDHS / N-Gqds / NF: The Ni-MOF / NF prepared by step (2) was submerged in the N-Gqds aqueous solution obtained by 35 ml of step (1) for 30 minutes, adding 0.12 g. Ga (NO 3 ) 2 • 6h 2 O and 0.3 g of urea, stirred for 10 minutes to form a uniform solution; transfer the solution to a 50 mL liner into polytetrafluoroethylene stainless steel autoclave, heated under 120 ° C for 5 hours, water and ethanol rinse several times NiGA-LDHS / N-Gqds / NF was obtained after 24 hours at 60 ° C. Calculated, the quality of NiGA-LDHS / N-Gqds on foam nickel is about 1.5 mg · cm -2.

[0033] As a reference, NIGA-LDHS / NF is prepared from the same method as described above.

[0034] figure 1 It is the XRD spectrum prepared by Ni-Mof / NF, NiGA-LDHS / NF and NiGA-LDHS / N-GqDS / NF; figure 1 It can be seen that NiGA-LDHS / N-GqDS / NF in Ni-mof diffraction peaks is good, which proves that Ni-MOF is successfully loaded on foam nickel; 11.3˚, 22.8 ˚, 34.4 ˚, 38.9˚, 60.0 ˚ and 61.2 ˚ of the diffraction angle corresponding to NiGa-LDHS (003), (006), (012), (013), (110), and (113) planes; visible, NIGA All diffraction peaks of -LDHS / N-GQDS / NF are consistent with NIGA-LDHS, while N-GQDS is not visible in the XRD spectrum due to the low N-Gqds content.

[0035] figure 2 The SEM map of Ni-MOF / NF, NiGA-LDHS / NF and NiGA-LDHS / N-Gqds / NF is prepared; in the figure, A is Ni-Mof / NF, B is NiGA-LDHS / NF, C is NIGA-LDHS / N-GQDS / NF; figure 2 It can be seen that Ni-MOF / NF is uniformly dispersed, and the particle diameter is about 150 nm; NiGA-LDHS / NF, NiGA-LDHS / N-Gqds / NF is nano-stranded composition; visible introduction After N-Gqds, the overall hierarchy has no significant change, but the NiGA-LDHS / N-GqDS / NF surface becomes rough, and the thickness of the nanoform is significantly increased. The increase in thickness increases the surface area, and the reactive site is increased, and the capacitance is increased, and the electrochemical performance is improved.

[0036] Example 2

[0037] In the case where other conditions are guaranteed, NiGA-LDHS / N-Gqds-X / NF, X is the concentration of N-Gqds an aqueous solution of N-Gqds. The comparative experiment is the same as the preparation method described in Example 1, and the difference is that the concentration of the N-Gqds aqueous solution in step (3) is from 1 mg · ml. -1 Replace 2, 3, 4 and 5 mg · ml, respectively -1.

[0038] image 3 The CV map of NiGA-LDHS / N-GqDS-X / NF was prepared in Example 2; Figure 4 Is a GCD map of Ni-Mof, NiGA-LDHS and NiGA-LDHS / N-GQDS-X / NF; image 3 It can be seen that when N-GQDS aqueous solution concentration is 2 mg · ml -1 NiGA-LDHS / N-GqDS-2 / NF performance was best. Depend on Figure 4 It can be seen that the prepared NiGA-LDHS / N-Gqds-2 / NF is the longest compared to other, and NiGA-LDHS / N-GQDS-2 / NF is found to be 1 A · g after calculation by the capacitor. -1 The specific capacitor is 2079 f · g -1 And the capacitance of NIGA-LDHS / N-GQDS-5 / NF is 882 f · g -1. NIGA-LDHS / NF in current density is 1 A · g -1 The specific capacitor is 928 f · g -1 The result indicates that the electrode material is significantly improved by the electrode material after the introduction of N-Gqds.

[0039] Example 3

[0040] In this example, a CO-MOF-derived carbon nanofed (Carbon NSS) loaded on the carbon cloth is prepared. 0.004mol co (NO) 3 ) 2 • 6h 2 O and 0.032 mol 2-mi were dissolved in 80 mL distilled water, respectively, poured 2-mi aqueous solution into Ni (NO) 3 ) 2 • 6h 2 O Aqueous solution is stirred for 10 minutes to obtain a mixed solution, then cut into 1 × 3 cm 2 The carbon cloth was placed in the above mixed solution for 2 hours, was washed several times with water and ethanol, 60 ° C for 5 hours, and the obtained Co-MOF was 5 ° C under the AR atmosphere. -1 Heating to 930 ° C for 2 hours, prepared to obtain CO-MOF-derived carbon nanoflakes. The resulting CO-MOF-derived carbon nanofold as an asymmetric supercapacitor. Evaluation of electrochemical properties in the CHI660E type electrochemical workstation (purchased from Shanghai Chenhua Instrument Co., Ltd.), under the three electrode system, NiGA-LDHS / N-GQDS / NF electrode material prepared in Example 1 as a work The electrode is evaluated as a reference electrode as a reference electrode in a Hg / HGO electrode, and the platinum sheet is evaluated as a pair of electrodes to the electrode material at a range of 0 to 0.5 V. And through the capacitance formula of electrode materials: C s = IT / MΔT calculates a comparison capacitor. The filter paper in which NiGA-LDHS / N-Gqds-2 / NF is positive is positive, and the carbon NSS is filtered into an asymmetric supercapacitor niGA-LDHS / N-GQDS / NF ///// CarbonNSS evaluates the performance of the device under the two electrode system.

[0041] Figure 5 It is a GCD curve for assembled asymmetric supercapacitors; it can be seen from the figure that the assembled asymmetric supercapacitor is 1A · g in current density -1 In the case of a specific capacitor 394 f · g -1. After testing, the capacitor can successfully light a plurality of LEDs, showing NiGA-LDHS / N-GqDS / NF as the actual application performance of the electrode material.