CN114360922A - Ag/g-C3N4Composite material and electrode material prepared from same - Google Patents
Ag/g-C3N4Composite material and electrode material prepared from same Download PDFInfo
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- CN114360922A CN114360922A CN202210046796.9A CN202210046796A CN114360922A CN 114360922 A CN114360922 A CN 114360922A CN 202210046796 A CN202210046796 A CN 202210046796A CN 114360922 A CN114360922 A CN 114360922A
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- 239000007772 electrode material Substances 0.000 title claims abstract description 44
- 239000000463 material Substances 0.000 title claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 40
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 16
- 239000011230 binding agent Substances 0.000 claims abstract description 13
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 13
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 11
- 239000001103 potassium chloride Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 8
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims abstract description 8
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 8
- 230000001376 precipitating effect Effects 0.000 claims abstract description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000003837 high-temperature calcination Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 10
- 230000001351 cycling effect Effects 0.000 abstract description 5
- 239000003990 capacitor Substances 0.000 description 25
- 239000000047 product Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 6
- 238000007600 charging Methods 0.000 description 5
- 238000007599 discharging Methods 0.000 description 5
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses an Ag/g-C3N4 composite material and an electrode material prepared from the same, wherein the electrode material is prepared from Ag/g-C3N4The composite material, the conductive carbon black and the binder. The preparation method comprises the steps of adding melamine and cyanuric acid into water, stirring, precipitating, separating and drying to obtain melamine-cyanuric acid supermolecules, mixing and grinding the supermolecules with potassium chloride, then calcining at high temperature to obtain g-C3N4The cubes are dispersed in silver nitrate solution and fully stirred, and are dried and then calcined at high temperature to obtain Ag/g-C3N4And finally, adding the powdery conductive carbon black and the binder into the composite material, and mixing to obtain the electrode material of the supercapacitor. The invention has higher specific capacitance, better rate performance and cycling stability, and can greatly improve the stability of the material. Has good application prospect.
Description
Technical Field
Hair brushRelates to the technical field of super capacitor electrode materials, in particular to Ag/g-C3N4Composite materials and electrode materials made therefrom.
Background
The development of clean energy and new technology for energy conversion and storage is a fundamental scheme for solving the problem that the current fossil energy is gradually exhausted. Among them, the super capacitor is an energy storage technology between a conventional capacitor and a rechargeable battery, having high power density and high energy density. In addition, the super capacitor has the characteristics of quick charging and discharging, high efficiency, no environmental pollution, long cycle life, wide working temperature range and high safety. The electrode material is the most important part of the super capacitor, and the electrochemical performance of the electrode material directly determines the performance of the super capacitor, so the design and preparation of the electrode material are the key for obtaining the high-performance super capacitor. g-C3N4The graphene-like carbon nitride film has a graphene-like structure, is a two-dimensional carbon nitride, and has a high specific surface area, a rich pore structure and high electrical conductivity. However, use of g-C alone3N4When used as an electrode material of a super capacitor, the material has poor performance (for example, low rate performance and low capacitance under high current density). Therefore, how to overcome the above-mentioned drawbacks is to develop g-C3N4An important issue for the base electrode material. Chinese patent document CN 103745836B discloses and reports a g-C3N4The/carbon quantum dot composite material has low conductivity and is still unsatisfactory.
Disclosure of Invention
The present invention is directed to overcoming the above-mentioned deficiencies in the prior art and providing a Ag/g-C alloy3N4A composite material.
Another object of the present invention is to provide a catalyst using Ag/g-C3N4The electrode material is made of the composite material, and is a high-rate super capacitor electrode material.
The purpose of the invention is realized by the following technical scheme:
Ag/g-C3N4A composite material produced by the following stepsPreparing to obtain:
step 1, adding melamine and cyanuric acid into water at room temperature, stirring, wherein the molar ratio of the melamine to the cyanuric acid is 1:1, centrifugally separating, precipitating, and drying to obtain a dried product which is a melamine-cyanuric acid supermolecule material;
step 3, g-C obtained in the step two3N4Dispersing the cubes in silver nitrate solution, fully stirring at room temperature, drying, and calcining at high temperature in nitrogen atmosphere to obtain Ag/g-C3N4A composite material.
In a further design scheme of the invention, in the step 1, the stirring time is 12-24 hours, and the drying temperature is 60-70 ℃.
In a further design scheme of the invention, the high-temperature calcination in the step 2 is carried out at the temperature of between 525 and 575 ℃ for 3 to 4 hours.
In a further design scheme of the invention, the high-temperature calcination temperature in the step 3 is 500-550 ℃, and the calcination process is 5 DEGoThe temperature is raised at the temperature raising rate of C/min, and the calcining time is 4 hours.
A high-rate super capacitor electrode material is prepared from Ag/g-C3N4The composite material is prepared by mixing the conductive carbon black and the binder.
In a further embodiment of the invention, Ag/g-C3N4The mass ratio of the composite material, the conductive carbon black and the binder is 8-10:1: 1.
Compared with the prior art, the invention has the following beneficial effects:
Ag/g-C in the high-rate super capacitor electrode material3N4The composite material not only shows higher capacitance, but also has better rate capability. At the same time, Ag/g-C3N4The composite material also has a very high degree of strengthThe capacitance value of the capacitor can be kept high for 2500 cycles under the condition of high current density.
The invention utilizes Ag to modify g-C3N4Nanocubes, such homogeneous cuboids Ag/g-C3N4The composite material is reported for the first time. Ag/g-C3N4The composite material has high rate performance and high cycling stability.
The preparation method of the high-rate super capacitor electrode material is simple and easy to implement, few in raw materials, short in flow, low in equipment dependence and suitable for industrial large-scale production and application, and only needs a simple preparation process.
Drawings
FIG. 1 is Ag/g-C in example3N4Scanning electron microscopy of the composite;
FIG. 2 is Ag/g-C in example3N4An X-ray diffraction pattern of the composite;
FIG. 3 is a graph of capacitance values of electrode materials of a high-rate supercapacitor at different current densities in examples;
FIG. 4 is a graph of 2500 cycles of the electrode material of the high-rate supercapacitor in the example under a current density of 1mA/cm 2.
Detailed Description
The invention is further explained below with reference to the drawings and examples.
Example 1:
preparation of Ag/g-C3N4Composite material
Adding 0.01 mol of melamine and 0.01 mol of cyanuric acid into 50 mL of water, stirring at room temperature for 24 hours, centrifuging the precipitate, and precipitating at 60%oAnd C, drying, wherein the dried product is melamine-cyanuric acid supermolecule. 1g of melamine-cyanuric acid supramolecules and 0.5g of potassium chloride were ground homogeneously. Placing into crucible with cover in tube furnace 550oCalcining for 4 hours at a temperature rising speed of 5oC/min, washing to remove redundant potassium chloride, and drying to obtain g-C3N4A cube. Mixing the above-mentioned 0.2 g g-C3N4Cubic samples were dispersed in 20 mL of 0.1 g/L silver nitrate solution and placed in the chamberStirred at room temperature for 6 hours and then at 60 deg.CoAnd C, drying for 12 hours. The resulting sample was placed in a quartz tube and heated under a nitrogen atmosphere at 5 deg.CoC/min heating rate in a tube furnace at 500oCalcining the C for 4 hours to obtain the product of Ag/g-C3N4A composite material.
For Ag/g-C3N4The composite material is subjected to electron microscope scanning and X-ray diffraction scanning, and Ag/g-C can be observed3N4The morphology and phase composition of the composite material are shown in FIGS. 1 and 2, and from FIG. 1, Ag/g-C prepared in this example3N4The specification and size of the composite material are as follows: a cube with a ridge length of about 400 nm. Ag is a particle with extremely small particle size and is uniformly distributed on cubic g-C3N 4. As can be seen from FIG. 2, the sample prepared in this example was at 13.0oAnd 27.4oCharacteristic peak pair of (1) corresponds to g-C3N4At the (100) and (002) planes of (A) at 38.0oThe samples prepared in this example are illustrated by the phase pure g-C for the (111) side of Ag3N4And Ag.
Preparation of electrode material of super capacitor
Taking Ag/g-C3N4The composite material is prepared by adding proper amount of powdered conductive carbon black and a binder, wherein the binder is polyvinylidene fluoride emulsion dissolved in 1-methyl-2-pyrrolidone, and Ag/g-C3N4The mass ratio of the composite material to the conductive carbon black to the binder is 8:1:1, and the mixture is mixed to obtain a viscous slurry-shaped supercapacitor electrode material.
A three-electrode system is adopted for testing a supercapacitor electrode material, a saturated calomel electrode is used as a reference electrode, a platinum wire is used as a counter electrode, the supercapacitor electrode material is used as a working electrode, cyclic voltammetry testing and charging and discharging testing are carried out on an electrochemical workstation CHI660D, and the capacitance value of the supercapacitor electrode material is calculated.
Referring to FIG. 3, it can be seen that the current density is 0.05 mA/cm2Has a capacitance value of 10.4 mF/cm at a current density of2At 1mA/cm2Under the condition of high current density, the capacitance value of the capacitor is 7.8 mF/cm2And the capacitance value is only reduced by 25% under the condition that the current density is improved by 20 times, and the high-capacitance-ratio capacitor has good rate-ratio performance.
Referring to FIG. 4, it can be seen that the current density is 1mA/cm2The capacity retention rate of the electrode material is about 99.8% after the electrode material is cycled for 2500 times under the condition of high current density, which shows that the obtained electrode material has stable cycling stability and is suitable for charging and discharging under the condition of high current.
Example 2:
preparation of Ag/g-C3N4Composite material
Adding 0.01 mol of melamine and 0.01 mol of cyanuric acid into 50 mL of water, stirring at room temperature for 12 hours, centrifuging the precipitate, and precipitating at 70%oAnd C, drying, wherein the dried product is melamine-cyanuric acid supermolecule. 1g of melamine-cyanuric acid supramolecules and 0.5g of potassium chloride were ground homogeneously. Put into a crucible with a cover in a tube furnace 575oCalcining for 3 hours at a temperature rise rate of 5oC/min, washing to remove redundant potassium chloride, and drying to obtain g-C3N4A cube. Mixing the above-mentioned 0.2 g g-C3N4Cubic samples were dispersed in 20 mL of 0.1 g/L silver nitrate solution and stirred at room temperature for 6 hours, then at 60oAnd C, drying for 12 hours. The resulting sample was placed in a quartz tube and heated under a nitrogen atmosphere at 5 deg.CoC/min heating rate in a tube furnace at 500oCalcining the C for 4 hours to obtain the product of Ag/g-C3N4A composite material.
Preparation of electrode material of super capacitor
Taking Ag/g-C3N4The composite material is prepared by adding proper amount of powdered conductive carbon black and a binder, wherein the binder is polyvinylidene fluoride emulsion dissolved in 1-methyl-2-pyrrolidone, and Ag/g-C3N4The mass ratio of the composite material to the conductive carbon black to the binder is 9:1:1, and the super capacitor electrode material is obtained after mixing.
Through tests, the capacitance value of the electrode material of the super capacitor prepared in the embodiment 2 is only reduced by 27% under the condition that the current density is increased by 20 times, and the electrode material has better rate performance.
Through testing, the electrode material of the super capacitor prepared in the example 2 is 1mA/cm2The capacity retention rate of the obtained capacitor is about 99.6 percent after being cycled for 2500 times under the condition of high current density, which shows that the obtained electricityThe electrode material has stable cycling stability and is suitable for charging and discharging under the condition of large current.
Example 3:
preparation of Ag/g-C3N4Composite material
Adding 0.01 mol of melamine and 0.01 mol of cyanuric acid into 50 mL of water, stirring at room temperature for 24 hours, centrifuging the precipitate, and precipitating at 60%oAnd C, drying, wherein the dried product is melamine-cyanuric acid supermolecule. 1g of melamine-cyanuric acid supramolecules and 0.5g of potassium chloride were ground homogeneously. Placing in a crucible with a cover in a tube furnace 525oCalcining for 4 hours at a temperature rising speed of 5oC/min, washing to remove redundant potassium chloride, and drying to obtain g-C3N4A cube. Mixing the above-mentioned 0.2 g g-C3N4Cubic samples were dispersed in 20 mL of 0.1 g/L silver nitrate solution and stirred at room temperature for 6 hours, then at 60oAnd C, drying for 12 hours. The resulting sample was placed in a quartz tube and heated under a nitrogen atmosphere at 5 deg.CoC/min heating rate in tube furnace at 550oCalcining the C for 3 hours to obtain the product of Ag/g-C3N4A composite material.
Preparation of electrode material of super capacitor
Taking Ag/g-C3N4The composite material is added with proper amount of powdered conductive carbon black and adhesive, the adhesive is polytetrafluoroethylene emulsion dissolved in 1-methyl-2-pyrrolidone, Ag/g-C3N4The mass ratio of the composite material to the conductive carbon black to the binder is 10:1:1, and the super capacitor electrode material is obtained after mixing. Through tests, the capacitance value of the electrode material of the super capacitor prepared in the embodiment 3 is only reduced by 26% under the condition that the current density is increased by 20 times, and the electrode material has better rate performance. The electrode material of the super capacitor prepared in the example 3 is 1mA/cm2The capacity retention rate of the electrode material is about 99.7% after the electrode material is cycled for 2500 times under the condition of high current density, which shows that the obtained electrode material has stable cycling stability and is suitable for charging and discharging under the condition of high current.
The above are preferred embodiments of the present invention, and all changes made according to the technical scheme of the present invention that produce functional effects do not exceed the scope of the technical scheme of the present invention belong to the protection scope of the present invention.
Claims (6)
1. Ag/g-C3N4The composite material is characterized in that the Ag/g-C3N4The composite material is prepared by the following steps:
step 1, adding melamine and cyanuric acid into water at room temperature, stirring, wherein the molar ratio of the melamine to the cyanuric acid is 1:1, centrifugally separating, precipitating, and drying to obtain a dried product which is a melamine-cyanuric acid supermolecule material;
step 2, mixing and grinding the melamine-cyanuric acid supramolecular material obtained in the step one and potassium chloride uniformly according to the mass ratio of 2:1, calcining at high temperature, washing to remove redundant potassium chloride, and drying to obtain g-C3N4A cube;
step 3, g-C obtained in the step two3N4Dispersing the cubes in silver nitrate solution, fully stirring at room temperature, drying, and calcining at high temperature in nitrogen atmosphere to obtain Ag/g-C3N4A composite material.
2. Ag/g-C according to claim 13N4The composite material is characterized in that in the step 1, the stirring time is 12-24 hours, and the drying temperature is 60-70 ℃.
3. Ag/g-C according to claim 13N4The composite material is characterized in that the high-temperature calcination temperature in the step 2 is 525-575 ℃, and the calcination time is 3-4 hours.
4. Ag/g-C according to claim 13N4The composite material is characterized in that the high-temperature calcination temperature in the step 3 is 500-550 ℃, and 5 ℃ is used in the calcination processoAnd (3) heating at the heating rate of C/min, wherein the calcining time is 3-4 hours.
5. High-rate super powerA container electrode material, characterized in that the supercapacitor electrode material is made of Ag/g-C in claim 13N4The composite material is prepared by mixing the conductive carbon black and the binder.
6. The high-rate supercapacitor electrode material according to claim 6, wherein the Ag/g-C3N4The mass ratio of the composite material, the conductive carbon black and the binder is 8-10:1: 1.
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| CN115959635A (en) * | 2022-12-13 | 2023-04-14 | 山东大学 | Monoatomic transition metal doped carbon nitride quantum dot, and chemical cutting preparation method and application thereof in water phase |
| WO2023236564A1 (en) * | 2022-06-07 | 2023-12-14 | 南通海星电子股份有限公司 | Preparation method for high-specific-surface-area high-dielectric sintered foil |
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| CN115959635A (en) * | 2022-12-13 | 2023-04-14 | 山东大学 | Monoatomic transition metal doped carbon nitride quantum dot, and chemical cutting preparation method and application thereof in water phase |
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