CN113517143B - Composite electrode material and preparation method and application thereof - Google Patents
Composite electrode material and preparation method and application thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to the technical field of energy material preparation, and particularly relates to a composite electrode material and a preparation method and application thereof. The invention adds Ni (NO) on the foamed nickel 3 ) 2 •6H 2 The porous Ni-MOF/NF prepared by using O and 2MI as raw materials has excellent mechanical properties, a staggered conductive network and rapid electron transmission. The prepared Ni-MOF/NF is put into N-GQDs solution for soaking, the N-GQDs have higher conductivity, the wettability of electrolyte is improved due to doping of a large number of nitrogen functional groups, and the high-performance NiGa-LDHs/N-GQDs/NF composite electrode material is prepared after etching by adding gallium ions. Not only is beneficial to the reaction of electrolyte ions and active materials, but also reduces the impedance of the materials and improves the cycling stability. The invention is used as the anode material to assemble the asymmetric super capacitor with ultrahigh power density and energy density, and provides an effective way for constructing a novel electrode material with high energy storage density, good cycle performance and good power density.
Description
Technical Field
The invention belongs to the technical field of energy material preparation, and particularly relates to a composite electrode material and a preparation method and application thereof.
Background
With the development of global economy, fossil fuels are largely burned, and the development of clean energy and related energy storage devices is imminent. Among the numerous energy storage devices, supercapacitors are considered to be one of the most promising clean energy storage devices to overcome the world energy crisis due to their advantages of superior power density, fast charging and discharging processes, excellent cycling stability, wide operating temperature range, environmental protection, and easy preparation. The super capacitor mainly comprises an electrode material and an electrolyte, so that the performance of the electrode material is a key influencing factor among a plurality of factors influencing the performance of the super capacitor, and is also a key and breakthrough difficulty of the current research. Research and development of novel electrode materials with low cost and high performance are the focus of attention and the main research direction of future researchers.
In the existing nanostructure, the two-dimensional nanosheet has a larger specific surface area and abundant exposed active sites, so that the two-dimensional nanosheet receives more and more attention in the field of energy storage of the supercapacitor. Layered double hydroxide compounds (LDHs) have the characteristics of abundant sources, low toxicity, high theoretical capacitance, better topological composition, easily-regulated multi-metal cations and the like, and become one of two-dimensional layered electrode materials which are widely concerned in recent years. Although LDHs can provide a higher specific capacitance, there are problems of poor stability and low intrinsic conductivity due to structural degradation of electrode materials during redox reactions.
The Metal Organic Frameworks (MOFs) have the characteristics of adjustable pore diameter, stable porous structure, large specific surface area and the like, are one of the widely applied bifunctional materials, and can be used as sacrificial templates and precursors of various ideal nano electrode materials such as metal hydroxides, metal oxides, metal sulfides and the like. In recent years, porous LDHs prepared from MOFs have received increasing attention in terms of their clear geometry, ultra-high surface area, and tunable pore size. LDHs based on macroporous MOFs can improve the interlayer ion flow efficiency and effectively reduce the ion transport resistance. However, MOFs-derived LDHs suffer from agglomeration. The Graphene Quantum Dots (GQDs) are a novel zero-dimensional carbon nanomaterial, and not only have the graphene properties of high electron transfer speed, large surface area and the like, but also have good biocompatibility such as excellent quantum confinement, edge effect and the like. These characteristics have led GQDs to receive extensive attention from researchers in recent years. At present, no research report about in-situ encapsulation of N-GQDs quantum dots on MOF derived NiGa-LDHs electrode materials is found.
Disclosure of Invention
In view of this, the present invention aims to provide a NiGa-LDHs/N-GQDs/NF composite electrode material, a preparation method and applications thereof. The composite electrode material can be used as an anode material, and a Co-MOF derived carbon nanosheet is used as a cathode material to be assembled into an asymmetric supercapacitor. A new way is opened for the design of nitrogen-doped graphene quantum dot hybrid electrode derived LDHs based on MOF packaging, and the method can be applied to the field of high-performance super capacitor energy storage.
In order to realize the purpose, the invention adopts the following technical scheme:
the invention provides a NiGa-LDHs/N-GQDs/NF composite electrode material, which takes two-dimensional Ni-MOF growing on foam Nickel (NF) as a supporting framework, loads nitrogen-doped graphene quantum dots on the supporting framework, and etches the nitrogen-doped graphene quantum dots through gallium ions to obtain the NiGa-LDHs/N-GQDs/NF composite electrode material.
The invention also provides a preparation method of the NiGa-LDHs/N-GQDs/NF composite electrode material, which comprises the following steps:
(1) placing citric acid and urea into water, performing ultrasonic dispersion, mixing, placing into a stainless steel autoclave with a polytetrafluoroethylene lining, performing heating reaction for a period of time, centrifuging a product, taking supernatant, drying to obtain N-GQD powder, and preparing into N-GQDs aqueous solution with a certain concentration for later use;
(2) rapidly pouring 2-MI aqueous solution into Ni (NO) 3 ) 2 •6H 2 Stirring the O aqueous solution to obtain a mixed solution, adding foamed nickel, immersing the foamed nickel into the mixed solution, carrying out aging reaction, washing the mixed solution for a plurality of times by using water and ethanol, and drying the washed mixed solution to obtain Ni-MOF/NF;
(3) putting the Ni-MOF/NF prepared in the step (2) into the N-GQDs aqueous solution obtained in the step (1) for soaking for a period of time, and adding Ga (NO) 3 ) 2 •6H 2 And stirring O and urea to form a uniform solution, transferring the solution into a stainless steel autoclave with a polytetrafluoroethylene lining, heating for reaction, washing the product with water and ethanol, and drying to obtain the NiGa-LDHs/N-GQDs/NF composite electrode material.
Further, the dosage relationship of the citric acid, the urea and the water in the step (1) is 0.42 g: 0.36-0.48 g: 30-36 mL.
The heating reaction in the step (1) is carried out at the temperature of 180-200 ℃ for 4-5 hours, and the drying temperature is 70-80 ℃.
The concentration of the N-GQDs aqueous solution in the step (1) is 1-5 mg/mL -1 。
The concentration of the 2-MI aqueous solution in the mixed solution in the step (2) is 0.0325-0.0475 g/mL -1 ，Ni(NO 3 ) 2 •6H 2 The concentration of the O aqueous solution was 0.015 g/mL -1 2-MI aqueous solution with Ni (NO) 3 ) 2 •6H 2 The volume ratio of the O aqueous solution is 1: 1.
The aging reaction time in the step (2) is 2-4 h, the drying temperature is 60-70 ℃, and the drying time is 4-5 h.
The aqueous solution of N-GQDs and Ga (NO) described in the step (3) 3 ) 2 •6H 2 The dosage relation of the O and the urea is 35-50 mL: 0.12 g: 0.3-0.6 g.
The heating reaction in the step (3) is carried out at the temperature of 120-150 ℃ for 4-5 h; the drying is carried out for 22-24 hours at the temperature of 60-70 ℃.
The invention also provides the application of the NiGa-LDHs/N-GQDs/NF composite electrode material in the preparation of asymmetric supercapacitors. The use is to use the NiGa-LDHs/N-GQDs/NF material as the anode material of the asymmetric super capacitor.
The invention also provides an asymmetric supercapacitor which is formed by assembling the NiGa-LDHs/N-GQDs/NF composite electrode material serving as a positive electrode material, filter paper soaked by KOH electrolyte serving as a diaphragm and Co-MOF derived carbon nanosheets serving as a negative electrode material.
Compared with the prior art, the invention has the beneficial effects that:
the invention uses normal temperature coprecipitation method to add Ni (NO) on the foam nickel 3 ) 2 •6H 2 And O and 2MI are used as raw materials to prepare porous Ni-MOF/NF with large specific surface area. Ni-MOF has excellent mechanical properties, an interlaced conductive network, and rapid electron transport. The prepared Ni-MOF/NF is put into N-GQDs solution for soaking, and the N-GQDs have higher conductivity due to dopingA large number of nitrogen functional groups improve the wettability of the electrolyte, and the high-performance NiGa-LDHs/N-GQDs/NF composite electrode material is prepared after etching by adding gallium ions. NiGa-LDHs derived from Ni-MOF adopts an MOF porous network structure as a conductive support with high specific surface area, high conductivity and high flexibility, and is used for anchoring N-GQDs and improving the specific capacitance of the N-GQDs, thereby improving the energy density of the super capacitor. The excellent performance of the method comes from introducing N-GQDs into layered NiGa-LDHs. The unique combination not only facilitates the reaction of electrolyte ions and active materials, but also reduces the impedance of the materials and improves the cycling stability. The composite material is used as a positive electrode material to assemble an asymmetric super capacitor (NiGa-LDHs/N-GQDs/NF// Carbon NSs), has ultrahigh power density and energy density, and can light a plurality of LEDs connected in parallel. The invention encapsulates quantum dots in the LDHs derived from the MOF, and provides an effective way for constructing a novel electrode material with high energy storage density, good cycle performance and good power density.
Drawings
FIG. 1 is an XRD spectrum of Ni-MOF/NF, NiGa-LDHs/NF and NiGa-LDHs/N-GQDs/NF prepared in example 1;
FIG. 2 is a SEM photograph of Ni-MOF/NF, NiGa-LDHs/NF and NiGa-LDHs/N-GQDs/NF prepared in example 1; in the figure, a is Ni-MOF/NF, b is NiGa-LDHs/NF, and c is NiGa-LDHs/N-GQDs/NF;
FIG. 3 is a CV diagram of NiGa-LDHs/N-GQDs-x/NF prepared in example 2;
FIG. 4 is a GCD plot of Ni-MOF, NiGa-LDHs and NiGa-LDHs/N-GQDs-x/NF;
figure 5 is a GCD curve for an assembled asymmetric supercapacitor.
Detailed Description
The present invention will be further described by the following examples, however, the scope of the present invention is not limited to the following examples. The present invention has been described generally and/or specifically with respect to materials used in testing and testing methods. The following examples are examples of experimental methods not indicating specific conditions, and the detection is usually carried out according to conventional conditions or according to the conditions recommended by the manufacturers. The reagents used in the following examples are all commercially available.
Example 1
(1) Preparation of N-GQDs: 0.42 g of citric acid and 0.36 g of urea in 30 mL of H 2 Carrying out ultrasonic dispersion in O for 2 hours, transferring the mixed solution into a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, and heating for 5 hours at 180 ℃; the resultant was centrifuged at 12000 rpm for 20 minutes, and the supernatant was dried at 80 ℃ to obtain N-GQD powder at a concentration of 1 mg/mL -1 The aqueous solution of N-GQDs is reserved;
(2) preparation of Ni-MOF/NF: 1.2g of Ni (NO) was added 3 ) 2 •6H 2 O and 2.6g 2-methylimidazole (2-MI) were dissolved in 80 mL of distilled water, and the 2-MI aqueous solution was poured into Ni (NO) quickly 3 ) 2 •6H 2 Stirring in O water solution for 10 min to obtain mixed solution, and cutting into pieces of 1 × 3cm 2 The foamed nickel is put into the mixed solution, aged for 2 hours, washed for a plurality of times by water and ethanol, and dried for 5 hours at 60 ℃ to obtain Ni-MOF/NF;
(3) preparation of NiGa-LDHs/N-GQDs/NF: putting the Ni-MOF/NF prepared in the step (2) into 35 mL of the N-GQDs aqueous solution obtained in the step (1) for soaking for 30 minutes, and adding 0.12 g of Ga (NO) 3 ) 2 •6H 2 O and 0.3 g of urea are stirred for 10 minutes to form a uniform solution; the solution was transferred to a 50mL stainless steel autoclave lined with Teflon, heated at 120 ℃ for 5 hours, rinsed several times with water and ethanol, and dried at 60 ℃ for 24 hours to give NiGa-LDHs/N-GQDs/NF. Calculated, the mass of NiGa-LDHs/N-GQDs loaded on the foamed nickel is about 1.5 mg cm -2 。
For reference, NiGa-LDHs/NF not added with N-GQDs was prepared in the same manner as described above.
FIG. 1 is an XRD spectrum of the prepared Ni-MOF/NF, NiGa-LDHs/NF and NiGa-LDHs/N-GQDs/NF; as can be seen from FIG. 1, the diffraction peak of Ni-MOF in NiGa-LDHs/N-GQDs/NF is well matched with that of Ni-MOF, which proves that Ni-MOF is successfully loaded on the foamed nickel; the diffraction angles from 11.3, 22.8, 34.4, 38.9, 60.0, and 61.2 < i > C </i > correspond to the (003), (006), (012), (013), (110), and (113) planes of NiGa-LDHs, respectively; as can be seen, all diffraction peaks of NiGa-LDHs/N-GQDs/NF are well matched with NiGa-LDHs, and the N-GQDs are not visible in an XRD spectrogram due to the low content of the N-GQDs.
FIG. 2 is a SEM image of the prepared Ni-MOF/NF, NiGa-LDHs/NF and NiGa-LDHs/N-GQDs/NF; in the figure, a is Ni-MOF/NF, b is NiGa-LDHs/NF, and c is NiGa-LDHs/N-GQDs/NF; as can be seen from FIG. 2, the Ni-MOF/NF is a nano sheet with uniform dispersion and uniform size, and the particle size is about 150 nm; NiGa-LDHs/NF and NiGa-LDHs/N-GQDs/NF are all formed by interleaving nano sheets; therefore, when the N-GQDs are introduced, the integral hierarchical structure is not obviously changed, but the surface of the NiGa-LDHs/N-GQDs/NF is rough, and the thickness of the nanosheets is obviously increased. The specific surface area is increased due to the increase of the thickness, the capacitance is increased due to the increase of reaction sites, and the electrochemical performance is improved.
Example 2
In this example, a comparative experiment was conducted to prepare NiGa-LDHs/N-GQDs-x/NF with different amounts of N-GQDs added, where x is the concentration of the aqueous solution of N-GQDs, while keeping other conditions unchanged. The comparative experiment was conducted in the same manner as the preparation described in example 1 except that the concentration of the aqueous solution of N-GQDs in step (3) was changed from 1 mg. multidot.mL -1 Respectively replaced by 2, 3, 4 and 5 mg/mL -1 。
FIG. 3 is a CV diagram of NiGa-LDHs/N-GQDs-x/NF prepared in example 2; FIG. 4 is a GCD diagram of Ni-MOF, NiGa-LDHs and NiGa-LDHs/N-GQDs-x/NF; as can be seen from FIG. 3, when the concentration of the aqueous solution of N-GQDs is 2 mg/mL -1 The prepared NiGa-LDHs/N-GQDs-2/NF has the best performance. As can be seen from FIG. 4, the discharge time of the prepared NiGa-LDHs/N-GQDs-2/NF is longest compared with other materials, and the NiGa-LDHs/N-GQDs-2/NF is found to be 1 A.g at the current density through capacitance calculation -1 Has a specific capacitance of 2079F g -1 While the NiGa-LDHs/N-GQDs-5/NF has a capacitance of 882 Fg -1 . The current density of NiGa-LDHs/NF is 1 A.g -1 Has a specific capacitance of 928F g -1 (ii) a The result shows that the specific capacitance of the electrode material is obviously improved due to the improvement of the conductivity after the introduction of the N-GQDs.
Example 3
Co-MOF derived Carbon nanosheets (Carbon NS) supported on Carbon cloth were prepared in this examples). 0.004 mol of Co (NO) 3 ) 2 •6H 2 O and 0.032 mol 2-MI were dissolved in 80 mL of distilled water, respectively, and the 2-MI aqueous solution was poured into Ni (NO) rapidly 3 ) 2 •6H 2 Stirring in O water solution for 10 min to obtain mixed solution, and cutting into 1 × 3cm 2 Aging the carbon cloth in the mixed solution for 2 hours, washing with water and ethanol for several times, drying at 60 ℃ for 5 hours, and subjecting the obtained Co-MOF to Ar atmosphere at 5 ℃ for min -1 Heating to 930 ℃ for 2 hours to prepare the Co-MOF derived carbon nano-sheet. The obtained Co-MOF derived carbon nanosheet was used as the negative electrode of an asymmetric supercapacitor. The evaluation of electrochemical performance was performed in a CHI660e type electrochemical workstation (purchased from Shanghai Chenghua instruments Co., Ltd.), and the capacity performance of the electrode material was evaluated in a three-electrode system under a voltage range of 0-0.5V using the NiGa-LDHs/N-GQDs/NF electrode material prepared in example 1 as a working electrode, a Hg/HgO electrode as a reference electrode, and a platinum sheet as a counter electrode. And by the capacitance formula of the electrode material: c s Specific capacitance is calculated by = It/m Δ t. And the performance of the device is evaluated under a two-electrode system by assembling the NiGa-LDHs/N-GQDs-2/NF as the anode, the filter paper soaked by 3M KOH electrolyte as the diaphragm and the Carbon NSs as the cathode.
FIG. 5 is a GCD curve for an assembled asymmetric supercapacitor; as can be seen from the figure, the assembled asymmetric supercapacitor has a current density of 1 A.g -1 In the case of (2), the specific capacitance is 394F g -1 . Through tests, the capacitor can successfully lighten a plurality of LEDs, and shows the practical application performance of the NiGa-LDHs/N-GQDs/NF as an electrode material.
Example 4
(1) Preparation of N-GQDs: 0.42 g of citric acid and 0.48 g of urea were added to 36mL of H 2 Carrying out ultrasonic dispersion in O for 2 hours, transferring the mixed solution into a 50mL stainless steel autoclave with a polytetrafluoroethylene lining, and heating for 4 hours at 200 ℃; the product was centrifuged at 12000 rpm for 20 minutes, and the supernatant was dried at 70 ℃ to give N-GQD powder prepared at a concentration of 1 mg mL -1 The aqueous solution of N-GQDs is reserved;
(2) preparation of Ni-MOF/NF: 1.2g of Ni (NO) 3 ) 2 •6H 2 O, 3.8g of 2-methylimidazole (2-MI) were dissolved in 80 mL of distilled water, respectively, and the 2-MI solution was poured into Ni (NO) quickly 3 ) 2 •6H 2 Stirring in O solution for 10 min to obtain mixed solution, and cutting into pieces of 1 × 3cm 2 The foamed nickel is put into the mixed solution, aged for 4 hours, washed for a plurality of times by water and ethanol, and dried for 4 hours at 70 ℃ to obtain Ni-MOF/NF;
(3) preparation of NiGa-LDHs/N-GQDs/NF: putting the Ni-MOF/NF prepared in the step (2) into 50mL of N-GQDs aqueous solution obtained in the step (1), soaking for 50 minutes, and adding 0.127 g of Ga (NO) 3 ) 2 •6H 2 O and 0.6g of urea are stirred for 12 minutes to form a uniform solution; the solution was transferred to a 50mL stainless steel autoclave lined with Teflon, heated at 150 ℃ for 4 hours, rinsed several times with water and ethanol, and dried at 70 ℃ for 22 hours to give NiGa-LDHs/N-GQDs/NF. Calculated, the mass of NiGa-LDHs/N-GQDs loaded on the foamed nickel is about 1.3mg cm -2 。
The above description is only an embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications, equivalents, flow charts, and other related technical fields that are made by the present invention will be included in the scope of the present invention.
Claims (10)
1. The NiGa-LDHs/N-GQDs/NF composite electrode material is characterized in that the composite electrode material takes two-dimensional Ni-MOF growing on foamed nickel as a supporting framework, nitrogen-doped graphene quantum dots are loaded on the supporting framework, and the supporting framework is etched by gallium ions to obtain the NiGa-LDHs/N-GQDs/NF composite electrode material.
2. A preparation method of a NiGa-LDHs/N-GQDs/NF composite electrode material is characterized by comprising the following steps:
(1) placing citric acid and urea into water, performing ultrasonic dispersion, mixing, placing into a stainless steel autoclave with a polytetrafluoroethylene lining, heating for reaction for a period of time, centrifuging a product, taking supernatant, drying to obtain N-GQD powder, and preparing the N-GQDs powder into an N-GQDs aqueous solution with a certain concentration for later use;
(2) rapidly pouring 2-MI aqueous solution into Ni (NO) 3 ) 2 •6H 2 Stirring the O aqueous solution to obtain a mixed solution, adding foamed nickel, immersing the foamed nickel into the mixed solution, carrying out aging reaction, washing the mixed solution for a plurality of times by using water and ethanol, and drying the washed mixed solution to obtain Ni-MOF/NF;
(3) putting the Ni-MOF/NF prepared in the step (2) into the N-GQDs aqueous solution obtained in the step (1) for soaking for a period of time, and adding Ga (NO) 3 ) 2 •6H 2 And stirring O and urea to form a uniform solution, transferring the solution into a stainless steel autoclave with a polytetrafluoroethylene lining, heating for reaction, washing the product with water and ethanol, and drying to obtain the NiGa-LDHs/N-GQDs/NF composite electrode material.
3. The method according to claim 2, wherein the citric acid, urea and water in step (1) are used in an amount of 0.42 g: 0.36-0.48 g: 30-36 mL.
4. The preparation method according to claim 2, wherein the temperature of the heating reaction in the step (1) is 180-200 ℃, the time is 4-5 h, and the drying temperature is 70-80 ℃; the concentration of the N-GQDs aqueous solution is 1-5 mg/mL -1 。
5. The method according to claim 2, wherein the concentration of the 2-MI aqueous solution in the mixed solution in the step (2) is 0.0325 to 0.0475 g/mL -1 ，Ni(NO 3 ) 2 •6H 2 The concentration of the O aqueous solution was 0.015 g/mL -1 2-MI aqueous solution with Ni (NO) 3 ) 2 •6H 2 The volume ratio of the O aqueous solution is 1: 1.
6. The preparation method according to claim 2, wherein the aging reaction time in the step (2) is 2-4 h, the drying temperature is 60-70 ℃, and the drying time is 4-5 h.
7. The method according to claim 2, wherein the aqueous solution of N-GQDs, Ga (NO) in step (3) 3 ) 2 •6H 2 The dosage relation of the O and the urea is 35-50 mL: 0.12 g: 0.3 to 0.6 g.
8. The preparation method according to claim 2, wherein the heating reaction in the step (3) is carried out at a temperature of 120 to 150 ℃ for 4 to 5 hours; the drying is carried out for 22-24 hours at the temperature of 60-70 ℃.
9. The use of the NiGa-LDHs/N-GQDs/NF composite electrode material of claim 1 in the preparation of anode materials in asymmetric supercapacitors.
10. An asymmetric supercapacitor, characterized in that the asymmetric supercapacitor is formed by assembling NiGa-LDHs/N-GQDs/NF composite electrode material of claim 1 as a positive electrode material, filter paper soaked by KOH electrolyte as a diaphragm, and Co-MOF derived carbon nanosheets as a negative electrode material.
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