CN112700967B - Cu with high specific capacity2-xNegative electrode material of Se super capacitor - Google Patents
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- 239000003990 capacitor Substances 0.000 title claims abstract description 29
- 239000007772 electrode material Substances 0.000 title description 13
- 239000010406 cathode material Substances 0.000 claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 42
- 229910052759 nickel Inorganic materials 0.000 claims description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 11
- 239000002033 PVDF binder Substances 0.000 claims description 8
- 239000006230 acetylene black Substances 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 239000011268 mixed slurry Substances 0.000 claims description 8
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 8
- 239000002105 nanoparticle Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005275 alloying Methods 0.000 claims description 4
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000004570 mortar (masonry) Substances 0.000 claims description 4
- 239000007773 negative electrode material Substances 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000012856 weighed raw material Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 12
- 239000003792 electrolyte Substances 0.000 abstract description 6
- 238000003487 electrochemical reaction Methods 0.000 abstract description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Inorganic materials [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 239000003575 carbonaceous material Substances 0.000 description 5
- 238000002484 cyclic voltammetry Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910021393 carbon nanotube Inorganic materials 0.000 description 2
- 239000002041 carbon nanotube Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 229910000474 mercury oxide Inorganic materials 0.000 description 2
- UKWHYYKOEPRTIC-UHFFFAOYSA-N mercury(ii) oxide Chemical compound [Hg]=O UKWHYYKOEPRTIC-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000010405 anode material Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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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
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- 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
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
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- Chemical & Material Sciences (AREA)
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Abstract
The invention disclosesCu with high specific capacity2‑xThe invention discloses a Se super capacitor cathode material and a manufacturing method thereof, relates to the field of super capacitors, and particularly relates to Cu2‑xThe Se material is applied to the field of super capacitors. The invention is applied to Cu of a super capacitor2‑xSe material has higher conductivity, provides faster kinetics for electrochemical reaction, reduces interfacial resistance between electrolyte and electrode, and shows 1040F g in strong alkaline aqueous solution‑1The specific capacity of (A). Shows Cu2‑xThe Se material is a potential super capacitor cathode material with excellent electrochemical performance.
Description
Technical Field
The invention relates to the field of super capacitors, in particular to Cu2-xThe Se material is applied to the field of super capacitors.
Background
The super capacitor is a novel energy storage device between the capacitor and the battery, stores energy by virtue of rapid and reversible adsorption/desorption or redox reaction on the surface or near the surface, has the characteristics of high specific capacity, long cycle life, large-current charge and discharge and the like, and is a research hotspot in the field of emerging green energy. Compared with the conventional secondary battery, the super capacitor has the excellent characteristics of high power density, short charging time, wide working temperature range, greenness, no pollution and the like, so that the super capacitor is expected to become a new-generation energy storage device. The electrode material is a core component of the super capacitor and is one of the most important factors determining the performance of the super capacitor. At present, the research on the positive electrode material is very extensive and has achieved good results, but the energy density of the super capacitor is still low due to the charge balance, so the negative electrode material with relatively low specific capacity has more research value. The carbon material as a traditional super capacitor cathode material has the advantage of high stability. Now thatIn the stage, a plurality of novel carbon materials such as activated carbon, graphene, carbon nanotubes and the like are applied to the super capacitor, and the carbon materials are characterized by large specific surface area and excellent stability. However, the specific capacity of these materials is quite undesirable. At present, the specific capacity of the activated carbon reported in the literature is only 100-120F g-1The specific capacity of the graphene is 100-230F g-1The specific capacity of the carbon nano tube is 20-160F g-1(adv. energy mater.2019.9.1900334). Therefore, it is urgent to find a super capacitor negative electrode material with high specific capacity.
Disclosure of Invention
The invention aims to provide novel Cu with high specific capacity2-xAnd (3) Se super capacitor cathode material. Cu2-xSe material has higher conductivity, provides faster kinetics for electrochemical reaction, reduces interfacial resistance between electrolyte and electrode, and shows 1040F g in strong alkaline aqueous solution-1The specific capacity of (A).
In order to achieve the purpose, the technical scheme of the invention is Cu with high specific capacity2-xThe Se super capacitor cathode material is characterized in that x is more than or equal to 0.1 and less than or equal to 0.2.
Further, Cu with high specific capacity2-xThe manufacturing method of the Se supercapacitor negative electrode material comprises the following steps:
step 1: according to Cu2-xThe stoichiometric ratio of Se, wherein x is more than or equal to 0.1 and less than or equal to 0.2, Cu and Se are weighed in an argon atmosphere, and the weighed raw materials are put into a nodular graphite tank filled with grinding balls and sealed; putting the ball milling tank filled with the raw materials into a high-energy ball mill for ball milling for 5-10h for alloying to obtain nano-sized powder;
step 2: cu obtained in the step 12-xSe powder is placed in an agate mortar, and Cu is added according to the mass ratio2-xSe powder: acetylene black: adding acetylene black and polyvinylidene fluoride into polyvinylidene fluoride according to the proportion of 7:2:1, dropwise adding 0.5-0.7 mL of N-methyl pyrrolidone, and fully grinding for 0.5 hour after dropwise adding is finished to obtain mixed slurry;
and step 3: uniformly scraping and coating the mixed slurry obtained in the step 2On the surface of foamed nickel subjected to ultrasonic treatment by deionized water and alcohol, the surface density of the foamed nickel is 290-430 g/m2, the pore diameter is 0.3-0.7 mm, the thickness is 1.5-2 mm, after blade coating is completed, the foamed nickel is placed in a vacuum drying oven for vacuum drying at the temperature of 50-60 ℃ for 12-24 hours, after natural cooling to room temperature, the foamed nickel is taken out and stands for 5-10min under the pressure of 10-15MPa, and the cathode material Cu of the supercapacitor is obtained2-xSe；
Further, in step 1, x is 0.2 or 0.15; the ball milling time in the step 2 is 10 h.
Further, in the step 3, the foam nickel is placed in a vacuum drying oven for vacuum drying for 24 hours at 55 ℃, after the temperature is naturally cooled to the room temperature, the foam nickel is taken out and stands for 5 minutes under the pressure of 15MPa, and the cathode material Cu of the super capacitor is obtained1.8Se or Cu1.85Se。
The beneficial technical effects are as follows: cu2-xSe material is one of the materials with the best thermoelectric property in a high-temperature section, and has the greatest characteristic of high electrical conductivity. The invention firstly puts Cu2-xThe Se material is applied to a super capacitor cathode material. Due to the high conductivity characteristic, the electrochemical reaction can be provided with faster kinetics, the interfacial resistance between the electrolyte and the electrode is reduced, and the electrochemical reaction shows that the interfacial resistance is up to 1040F g in a strong alkaline aqueous solution-1The specific capacity of the carbon material is far higher than that of the carbon material. Thus showing Cu2-xThe Se material is a potential super capacitor cathode material with excellent electrochemical performance. Standing for 5min under the pressure of 15MPa to improve the stability and firmness of the electrode; finally, the foam nickel is coated with a layer of Cu2-xSe super capacitor cathode material.
Drawings
FIG. 1 shows the electrode material Cu of the supercapacitor obtained in example 11.85Scanning Electron Microscope (SEM) image of Se;
FIG. 2 shows the electrode material Cu of the supercapacitor obtained in examples 1 and 21.85Se and Cu1.8X-ray diffraction pattern of Se. The characteristic peak of X-ray diffraction is well matched with a standard card, and the sample prepared in the embodiment is proved to be Cu1.85Se and Cu1.8Se super capacitorA device anode material;
FIG. 3 shows the electrode material Cu of the supercapacitor obtained in example 11.85Cyclic voltammograms of Se at different scanning speeds;
FIG. 4 shows the electrode material Cu of the supercapacitor obtained in example 11.85Constant current charge-discharge curve diagram of Se under different current densities;
Detailed Description
The following describes an embodiment of the present invention with reference to the drawings.
The first embodiment is as follows:
step 1: high-purity simple substances Cu and Se are used as starting materials, and Cu is in a stoichiometric ratio1.85Weighing Se, wherein x is 0.15, putting the weighed raw materials into a nodular graphite tank filled with grinding balls in an argon atmosphere, and sealing; putting the ball milling tank filled with the raw materials into a high-energy ball mill for ball milling for 10 hours to carry out alloying to obtain nano-sized powder;
step 2: cu obtained in the step 11.85Se powder is placed in an agate mortar according to Cu1.85Se powder: acetylene black: adding acetylene black and polyvinylidene fluoride into polyvinylidene fluoride according to the proportion of 7:2:1, dropwise adding 0.5-0.7 mL of N-methyl pyrrolidone, mixing all the materials, and then fully grinding for 0.5 hour to obtain mixed slurry;
and step 3: uniformly blade-coating the mixed slurry obtained in the step 2 on the surface of foamed nickel (the surface density of the foamed nickel is 290-430 g/m2, the pore diameter is 0.3-0.7 mm, and the thickness is 1.5-2 mm) subjected to ultrasonic treatment by using deionized water and alcohol, after the blade-coating is finished, placing the foamed nickel in a vacuum drying oven for vacuum drying at 55 ℃ for 24 hours, naturally cooling to room temperature, taking out the foamed nickel, and standing for 5 minutes under the pressure of 15MPa to obtain the cathode material Cu of the supercapacitor1.85Se。
And 4, step 4: adding the cathode material Cu of the super capacitor obtained in the step 31.85And carrying out electrochemical performance test by Se. The experiment used a three-electrode system: the working electrode is Cu1.85Se cathode material, reference electrode as mercury oxide electrode, counter electrode as platinum electrode, electrolyte as 3mol L-1Potassium hydroxide solution of (2).
Example stationCan be shown as Cu in figure 11.85Scanning Electron Microscope (SEM) picture of Se, showing Cu1.85Se exists in a mode of stacking nanoparticles, the nanoparticles are beneficial to full contact of electrode materials and electrolyte, and meanwhile, the ion/proton transfer and transmission distances can be shortened, so that the high-performance supercapacitor electrode materials can be obtained.
Example the result is Cu as shown in FIG. 21.85The X-ray diffraction pattern of Se corresponds to Cu at 26.66 °, 30.88 °, 44.23 °, 52.40 °, 54.91 ° and 64.34 ° respectively1.85The (111), (200), (220), (311), (222) and (400) crystal planes of the Se cubic system structure.
Example the resulting supercapacitor electrode Material Cu1.85The cyclic voltammograms of Se at different scan speeds are shown in figure 3. The voltage test range of the cyclic voltammetry is 0.2V to-1V, and the scanning speed is 1mv/s, 2mv/s, 5mv/s, 10mv/s and 20mv/s respectively. The cyclic voltammetry curves at all scanning speeds have obvious oxidation reduction peaks, which indicates that the electrode material Cu1.85The specific capacitance of Se is mainly pseudocapacitance. As the scan speed increased, the redox peak position gradually and slowly moved to both sides and the closed area gradually increased, and the shape of the cyclic voltammogram hardly changed, indicating good ion transport ability and fast kinetics.
Example the resulting supercapacitor electrode Material Cu1.85The constant current charge-discharge curve of Se at different current densities is shown in FIG. 4. Applied current densities of 2A g respectively-1、5A g-1、10A g-1、15A g-1And 20A g-1Charge and discharge curves at time. The voltage test window of the constant current charge and discharge of the experiment is-1V to 0V. As can be seen from the figure, the electrode material Cu1.85Se has an obvious discharge platform and conforms to the characteristics of pseudo-capacitance. The discharge time decreases with a gradual increase in current density, and the specific capacitance also gradually decreases. Current density of 2A g-1When the specific capacitance is maximum, 1040F g is reached-1This is the currently reported premium. Thus showing Cu1.85Se is a potential super capacitor cathode material with excellent electrochemical performance.
Example two:
step 1: high-purity simple substances Cu and Se are used as starting materials, and Cu is in a stoichiometric ratio1.8Weighing Se, wherein x is 0.2, putting the weighed raw materials into a nodular graphite tank filled with grinding balls in an argon atmosphere, and sealing; putting the ball milling tank filled with the raw materials into a high-energy ball mill for ball milling for 10 hours to carry out alloying to obtain nano-sized powder;
step 2: cu obtained in the step 11.8Se powder is placed in an agate mortar according to Cu1.8Se powder: acetylene black: adding acetylene black and polyvinylidene fluoride into polyvinylidene fluoride according to the proportion of 7:2:1, dropwise adding 0.5-0.7 mL of N-methyl pyrrolidone, mixing all the materials, and then fully grinding for 0.5 hour to obtain mixed slurry;
and step 3: uniformly blade-coating the mixed slurry obtained in the step 2 on the surface of foamed nickel (the surface density of the foamed nickel is 290-430 g/m2, the pore diameter is 0.3-0.7 mm, and the thickness is 1.5-2 mm) subjected to ultrasonic treatment by using deionized water and alcohol, after the blade-coating is finished, placing the foamed nickel in a vacuum drying oven for vacuum drying at 55 ℃ for 24 hours, naturally cooling to room temperature, taking out the foamed nickel, and standing for 5 minutes under the pressure of 15MPa to obtain the cathode material Cu of the supercapacitor1.8Se。
And 4, step 4: adding the cathode material Cu of the super capacitor obtained in the step 31.8And carrying out electrochemical performance test by Se. The experiment used a three-electrode system: the working electrode is Cu1.8Se cathode material, reference electrode as mercury oxide electrode, counter electrode as platinum electrode, electrolyte as 3mol L-1Potassium hydroxide solution of (2).
Example the result is Cu as shown in FIG. 21.8The X-ray diffraction pattern of Se corresponds to Cu at 26.79 °, 31.03 °, 44.46 °, 52.67 °, 55.21 ° and 64.69 ° respectively1.8The (111), (200), (220), (311), (222) and (400) crystal planes of the Se cubic system structure.
Claims (3)
1. Cu with high specific capacity2-xThe manufacturing method of the Se supercapacitor negative electrode material comprises the following steps:
step 1: according to Cu2-xThe stoichiometric ratio of Se, wherein x is more than or equal to 0.1 and less than or equal to 0.2, Cu and Se are weighed in an argon atmosphere, and the weighed raw materials are put into a ball milling tank filled with grinding balls and sealed; putting the ball milling tank filled with the raw materials into a high-energy ball mill for ball milling for 5-10h for alloying to obtain nano-sized powder;
step 2: cu obtained in the step 12-xSe powder is placed in an agate mortar, and Cu is added according to the mass ratio2-xSe powder: acetylene black: adding acetylene black and polyvinylidene fluoride into polyvinylidene fluoride according to the proportion of 7:2:1, dropwise adding 0.5-0.7 mL of N-methyl pyrrolidone, and fully grinding for 0.5 hour after dropwise adding is finished to obtain mixed slurry;
and step 3: uniformly blade-coating the mixed slurry obtained in the step 2 on the surface of foamed nickel subjected to ultrasonic treatment by deionized water and alcohol, wherein the surface density of the foamed nickel is 290-430 g/m2, the pore diameter is 0.3-0.7 mm, and the thickness is 1.5-2 mm, after the blade-coating is finished, placing the foamed nickel in a vacuum drying oven for vacuum drying at the temperature of 50-60 ℃ for 12-24 hours, naturally cooling to room temperature, taking out the foamed nickel, and standing for 5-10min under the pressure of 10-15MPa to obtain the cathode material Cu of the supercapacitor2-xSe。
2. The manufacturing method according to claim 1, wherein x =0.2 or 0.15 in step 1; the ball milling time in the step 2 is 10 h.
3. The manufacturing method of claim 1, wherein in the step 3, the foamed nickel is placed in a vacuum drying oven for vacuum drying at 55 ℃ for 24 hours, and after the temperature is naturally cooled to room temperature, the foamed nickel is taken out and stands for 5 minutes under the pressure of 15MPa to obtain the cathode material Cu of the super capacitor1.8Se or Cu1.85Se。
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| US20070163640A1 (en) * | 2004-02-19 | 2007-07-19 | Nanosolar, Inc. | High-throughput printing of semiconductor precursor layer by use of chalcogen-rich chalcogenides |
| CN105304905A (en) * | 2015-09-23 | 2016-02-03 | 合肥国轩高科动力能源有限公司 | Modified material for positive electrode of lithium ion battery and preparation method of modified material |
| CN105789350B (en) * | 2016-03-24 | 2017-03-29 | 陕西师范大学 | Exposure { 111 } crystal face Cu2Se/Cu2The preparation method of O superlattices sub-micro rice noodles |
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| CN108933257A (en) * | 2018-08-31 | 2018-12-04 | 浙江大学 | Cu as lithium ion battery electrode material2-xSe nano material and preparation method thereof |
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