CN115101351A - Composite positive electrode material NiSe of super capacitor with ultrahigh multiplying power 2 @CoSe 2 And construction thereof - Google Patents
Composite positive electrode material NiSe of super capacitor with ultrahigh multiplying power 2 @CoSe 2 And construction thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 38
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000003990 capacitor Substances 0.000 title claims abstract description 11
- 239000007774 positive electrode material Substances 0.000 title claims abstract description 7
- 238000010276 construction Methods 0.000 title claims description 5
- 230000009467 reduction Effects 0.000 claims abstract description 4
- 239000010405 anode material Substances 0.000 claims abstract description 3
- 238000004070 electrodeposition Methods 0.000 claims abstract 2
- 239000007772 electrode material Substances 0.000 claims description 35
- 239000003792 electrolyte Substances 0.000 claims description 7
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 5
- 238000004146 energy storage Methods 0.000 abstract description 3
- 150000002500 ions Chemical class 0.000 description 17
- 230000007547 defect Effects 0.000 description 8
- 239000011669 selenium Substances 0.000 description 8
- 150000003623 transition metal compounds Chemical class 0.000 description 8
- 239000011149 active material Substances 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 238000006479 redox reaction Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 150000001450 anions Chemical class 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 2
- 238000007600 charging Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005036 potential barrier Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 229940075397 calomel Drugs 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000010277 constant-current charging Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000004299 exfoliation Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052723 transition metal Inorganic materials 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
-
- 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
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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 a composite positive electrode material NiSe of an ultra-high magnification super capacitor 2 @CoSe 2 Belonging to the field of new energy storage. The invention adopts simple electrodeposition and reduction treatment to prepare NiSe rich in Se vacancy 2 @CoSe 2 Heterojunctions, and a specific interface semi-coherent matching relation exists between the heterojunctions; Vr-NiSe prepared by the invention 2 @CoSe 2 The composite material has ultrahigh rate performance, and the current density is increased to 250A g ‑1 The specific capacity of the material can still keep 60.4 percent of the original specific capacity, and the material provides a high-quality candidate anode material for constructing a new generation of high-performance super capacitor.
Description
Technical Field
The invention relates to the field of new energy storage, in particular to an ultra-high rate NiSe 2 @CoSe 2 A super capacitor composite anode material.
Technical Field
The super capacitor is a novel energy storage device developed in recent years, has the advantages of high power density, high charging speed, long cycle service life, wide working temperature range, good safety performance, environmental protection and the like, and has wide application prospect in the fields of new energy automobiles, micro communication equipment, heavy machinery, aerospace and the like (Chinese invention patent, application number 201810202685.6). It is well known that the performance of a supercapacitor is completely dependent on its electrode material. However, supercapacitors still lack high performance electrode Materials compared to rechargeable batteries, which severely limits their industrial production process (Energy & Environmental Science,2016,9,102-106.Advanced Energy Materials,2019,9, 1802928). Therefore, designing and constructing a novel electrode material with excellent electrochemical performance is of great significance for improving the energy density of the supercapacitor.
In recent years, researchers have often improved the charge storage capacity of supercapacitors by designing new cathode materials, which they have attempted to use NiMoO 4 ，CoNi-MOF，NiCoP/NiCo-OH，MoS 2 ,Fe 2 O 3 ，NiCoSe 2 And transition metal compounds are taken as positive electrode Materials mainly due to the advantages of higher theoretical specific capacitance, excellent oxidation-reduction property and electrochemical activity, abundant raw Materials, environmental friendliness, low price and the like (Nature Communications,2017,8,14264.Advanced Energy Materials,2017,7,1700294.Advanced Functional Materials,2018,28,1800036.Nature Nanotechnology,2015,10,313-318. Chinese patent application No. 201310058911.5; Chinese patent application No. 201611200095.7). However, these compounds have disadvantages of poor electron transport ability and low rate. In order to overcome the above problems, researchers often use carbon Materials with good conductivity and large specific surface area as a skeleton to be compounded with the carbon Materials, or compound two or more transition metal compounds (Advanced Energy Materials,2018,8,1702247.Nano Energy,2017,35,331-340.Energy&Environmental Science,2016,9,1299-1307.adv. energy mater.2016,6,1600341). Although the specific capacitance of the prepared composite electrode material is higher than that of a single active material, the rate performance of the composite electrode material cannot meet the requirement of a novel high-performance super capacitor, and the practical application of the composite electrode material in the super capacitor is greatly hindered. The reason for this is probably that the above-mentioned skeleton and active material are simply physically adsorbed and complexedWhen the electrode material is charged and discharged at a high current, ions in the electrolyte are rapidly embedded/released to generate obvious expansion/contraction of the volume of the electrode material, and meanwhile, the electrode material can generate a stress concentration phenomenon due to large alternating stress circulation, so that the active material is pulverized and even falls off from the surface of a framework, and the whole electrode structure is seriously collapsed; and for the previously reported constructed transition metal compound composite electrode material, due to anisotropic crystal growth and inherent lattice mismatch, such a heterogeneous interface is unstable, thereby causing active material exfoliation or ion transmission path interruption during discharge/charge. Therefore, how to construct a composite electrode material with high internal activity, strong electron transmission capability and specific interface lattice matching relationship, and systematically explore the influence rule of the composite electrode material on the rate capability of the electrode material is a huge challenge in the field and a bottleneck problem which must be overcome in future large-scale application of the supercapacitor.
Researches show that transition metal compounds with different energy levels can cause the change of an interface electronic structure, then a built-in electric field and two opposite charge distribution areas are generated on a heterogeneous interface of the transition metal compounds, and the generated built-in electric field greatly accelerates the ion migration rate, so that the rapid reaction kinetics are facilitated, the ion diffusion potential barrier is reduced, and the multiplying power performance is improved; at the same time, the specific space charge area generated also favours the ion adsorption, so that easier redox reactions can be carried out (adv. energy mater.2017,8,1.chem.sci.2021,12,6048701228). Vacancy engineering is considered to be an ideal technique for enhancing the electrochemical performance of transition metal compounds. On the one hand, the introduction of vacancies in the transition metal compound can create defect levels in the forbidden region, leading to a reduction of the forbidden band and a shift of the fermi level. Therefore, the anion vacancy can be used as a shallow donor, effectively regulate the electronic structure, and enhance the conductivity of the transition metal compound [ adv. mater.2020,32,1905923, ACS Nano 2018,12,1894]. On the other hand, the presence of vacancy defects interferes to some extent with the surrounding atoms, resulting in a reduction in their coordination number, inevitably producing a large number of exposed unsaturated dangling bonds in the vacancy portion, which can serve as strong adsorption sites for foreign ions or intermediate species, to serve as a site for the adsorption of foreign ions or intermediate speciesA more stable state of the system is achieved; meanwhile, a large number of VI element vacancy defects (namely sulfur or selenium vacancies) can be found, and the VI element vacancy defects are all provided with positive charges (proton states), so that abundant anions can be smoothly captured [ adv]. Thus, vacancies more readily trap electrolyte ions, and then provide a wide space for ion storage, further facilitating redox reactions. In addition, the vacancy defect can generate a profound influence on ion intercalation/delamination in the active material, reduce stress concentration and electrostatic repulsion between adjacent layers, directly serve as a 'highway' channel for accelerating ion migration, and effectively overcome diffusion barriers in the charge/discharge process. Therefore, it greatly improves the reaction kinetics and rate capability of the electrode material. In addition, the generated vacancy defects can increase the surface energy of the system, so that a large number of active centers are generated, more electrode materials are contacted with electrolyte ions to carry out redox reaction, and the specific capacity of the electrode materials is further improved. Thus, NiSe with rich Se vacancies and semi-coherent interfaces is constructed 2 @CoSe 2 The heterojunction is expected to greatly improve the rate capability of the composite cathode material.
Disclosure of Invention
The invention aims to overcome the defects of poor cycle stability and the like of a doped graphene @ transition metal phosphide composite electrode material.
The purpose of the invention is realized by the following technical scheme:
(1) NiSe rich in Se vacancy 2 @CoSe 2 Preparing a composite electrode material:
adding 10mmol L of -1 NiCl 2 ·6H 2 O，5mmol L -1 CoCl 2 ·6H 2 O，30mmol L -1 SeO 2 And 0.1mol L - 1 LiCl is uniformly mixed to be used as electrolyte and deposited for 10min under-0.8V to obtain NiSe 2 @CoSe 2 A heterojunction; then put it into 0.1mol L -1 KBH 4 Soaking in the solution for 10min to obtain NiSe containing abundant Se vacancy 2 @CoSe 2 Composite electrode material (Vr-NiSe) 2 @CoSe 2 )。
(2)Vr-NiSe 2 @CoSe 2 Electrochemical performance testing of the composite material:
first, a KOH solution having a concentration of 2M was prepared as an electrolyte solution, and then, Vr-NiSe was deposited 2 @CoSe 2 The composite electrode material, the Pt electrode and the calomel electrode are respectively used as a working electrode, a counter electrode and a reference electrode, and an electrochemical workstation is used for respectively testing constant current charging and discharging (GCD) and the like of the obtained composite electrode material to obtain the multiplying power characteristic of the composite electrode material.
The invention discloses Vr-NiSe 2 @CoSe 2 Compared with the existing electrode material, the composite electrode material has the advantages that:
(1) in the invention, NiSe is prepared 2 @CoSe 2 The novel composite electrode material has the characteristics of a semi-coherent interface (the interface mismatching degree is 13.5 percent), not only can generate a built-in electric field and two opposite charge distribution areas, greatly accelerates the ion migration rate and reduces the ion diffusion potential barrier, but also can ensure that the composite electrode material is not easy to fall off under the current in the charging and discharging process, thereby ensuring the integration of the structure and promoting the multiplying power performance of the composite electrode material.
(2) In the present invention, NiSe 2 @CoSe 2 A large number of Se vacancies are introduced, so that the electronic structure of the electrode material is regulated, the conductivity is improved, the ion adsorption capacity is increased, a rapid channel is provided for the diffusion of ions, and the reaction kinetics and the rate capability of the electrode material are greatly improved; in addition, the generated vacancy defects can increase the surface energy of the system, so that a large number of active centers are generated, more electrode materials are contacted with electrolyte ions to perform redox reaction, and the specific capacity of the electrode materials is improved.
Drawings
The invention is further explained below with reference to the drawings and examples.
FIG. 1 shows Vr-NiSe 2 @CoSe 2 SEM photograph of the composite material.
FIG. 2 shows Vr-NiSe 2 @CoSe 2 And NiSe 2 @CoSe 2 XRD pattern of the composite.
FIG. 3 is NiSe 2 @CoSe 2 Pure and pureNiSe 2 And CoSe 2 Se 3 dpxs profile of (c).
FIG. 4 shows Vr-NiSe 2 @CoSe 2 And NiSe 2 @CoSe 2 EPR profile of the composite.
FIG. 5 shows Vr-NiSe 2 @CoSe 2 The specific capacity of the composite material is along with the change curve of current density.
Detailed Description
Example 1
Vr-NiSe 2 @CoSe 2 Preparation of composite materials
First, 10mmol L of -1 NiCl 2 ·6H 2 O，5mmol L -1 CoCl 2 ·6H 2 O，30mmol L -1 SeO 2 And 0.1mol L -1 LiCl was mixed uniformly as an electrolyte, and the mixture was further mixed by 1cm -2 The graphite substrate, the Pt wire electrode and the saturated calomel are respectively used as a working electrode, a counter electrode and a reference electrode, the deposition voltage is controlled to be-0.8V, and deposition is carried out for 10min to obtain NiSe 2 @CoSe 2 A heterojunction; finally, it is placed in 0.1mol L -1 KBH 4 Soaking in the solution for 10min, taking out, and drying at 60 deg.C for 12h to obtain NiSe with abundant Se vacancy 2 @CoSe 2 Composite electrode material (Vr-NiSe) 2 @CoSe 2 ). Simultaneously, the same process is adopted to obtain NiSe 2 @CoSe 2 Pure NiSe 2 And CoSe 2 。Vr-NiSe 2 @CoSe 2 SEM photographs of the composite material are shown in fig. 1; Vr-NiSe 2 @CoSe 2 And NiSe 2 @CoSe 2 The XRD, Se 3d XPS and EPR characterization results of the composite material are shown in fig. 2, fig. 3 and fig. 4, respectively.
Vr-NiSe 2 @CoSe 2 Electrochemical performance testing of composite materials
By Vr-NiSe 2 @CoSe 2 The composite electrode material is a working electrode, the saturated calomel electrode is a reference electrode, the platinum wire electrode is a counter electrode to form a three-electrode system, and the working electrode is 2 mol.L -1 The change of the specific capacity with the current density was measured in the KOH solution of (1), as shown in FIG. 5, and it can be seen from FIG. 5 that when the current density was increased to 250Ag -1 Then, its specific capacity can still be60.4% of the original specific capacitance is kept, which indicates that the electrode material has ultrahigh rate performance.
Claims (3)
1. Composite positive electrode material NiSe of super capacitor with ultrahigh multiplying power 2 @CoSe 2 And the construction thereof, characterized in that: NiSe with rich Se vacancy is obtained by adopting one-step electrodeposition method and reduction treatment 2 @CoSe 2 The interface of the supercapacitor composite anode material is a typical semi-coherent interface and is combined by a chemical bond.
2. The ultra-high rate composite super capacitor positive electrode material NiSe according to claim 1 2 @CoSe 2 And the construction thereof, characterized in that: 10mmol L of the product was prepared -1 NiCl 2 ·6H 2 O，5mmol L -1 CoCl 2 ·6H 2 O，30mmol L -1 SeO 2 And 0.1mol L -1 LiCl mixed electrolyte is deposited for 10min under-0.8V to obtain NiSe 2 @CoSe 2 A heterojunction; then put it into 0.1mol L -1 KBH 4 Soaking in the solution for 10min to obtain NiSe containing abundant Se vacancy 2 @CoSe 2 (Vr-NiSe 2 @CoSe 2 )。
3. The ultra-high rate composite super capacitor positive electrode material NiSe according to claim 1 2 @CoSe 2 And the construction thereof, characterized in that: the composite electrode material has ultrahigh rate characteristic of 250Ag -1 The specific capacity can still maintain 60.4 percent of the original specific capacity.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115557473A (en) * | 2022-10-10 | 2023-01-03 | 浙江工业大学 | Preparation method of two-component nano heterojunction material with coherent growth characteristic |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115557473A (en) * | 2022-10-10 | 2023-01-03 | 浙江工业大学 | Preparation method of two-component nano heterojunction material with coherent growth characteristic |
| CN115557473B (en) * | 2022-10-10 | 2023-10-20 | 浙江工业大学 | Preparation method of double-component nano heterojunction material with coherent growth characteristics |
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