CN114360919A - Preparation method of high-performance electrode material with nano sea urchin structure - Google Patents
Preparation method of high-performance electrode material with nano sea urchin structure Download PDFInfo
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- 239000007772 electrode material Substances 0.000 title claims abstract description 37
- 241000257465 Echinoidea Species 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000008367 deionised water Substances 0.000 claims abstract description 22
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 9
- 239000006260 foam Substances 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 8
- 230000001351 cycling effect Effects 0.000 abstract description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 8
- 239000003990 capacitor Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 239000003792 electrolyte Substances 0.000 description 4
- 239000002070 nanowire Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000003245 coal Substances 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052976 metal sulfide Inorganic materials 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- -1 transition metal sulfide Chemical class 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005486 sulfidation Methods 0.000 description 1
- 238000005987 sulfurization reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
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Abstract
The invention belongs to the field of electrode material preparation, and relates to a preparation method of a high-performance electrode material with a nano sea urchin structure. The method comprises the following steps: pretreating foamed nickel, dissolving 2-6mmol of cobalt nitrate hexahydrate, 0.5-1.5g of ammonium fluoride and 0.5-2.0g of urea in 40-80ml of water, magnetically stirring for 20-45min, transferring the solution into a reaction kettle, preserving heat for 6-8h at the temperature of 100-120 ℃, naturally cooling to room temperature, and cleaning for 3-5 times by using absolute ethyl alcohol and deionized water to obtain a precursor; adding 6-9mmol of sodium sulfide into 50-60ml of deionized water, magnetically stirring for 45min, transferring the precursor into the reaction kettle, preserving heat for 4h at the temperature of 100-120 ℃, naturally cooling to room temperature, washing with absolute ethyl alcohol and deionized water for 3-5 times to obtain a sulfide sample, preserving heat for 12h at the temperature of 60 ℃, and drying. The method well improves the problems of specific capacitance, cycling stability and the like of the electrode material.
Description
Technical Field
The invention belongs to the field of electrode material preparation, and particularly relates to a preparation method of a high-performance electrode material with a nano sea urchin structure, which can be used in the related fields of batteries and the like.
Background
In recent years, the rapid development of the technology level makes our daily life change greatly. The vehicles, communication tools and living appliances used by people are changed over the ground due to the continuous development of science and technology,all of these advances have relied primarily on the development and utilization of energy, which plays a very important role in our daily lives. In ancient times, mankind has learned to drill wood and get fire in order to be able to eat cooked food, so that wood appears before the world as the earliest energy source that mankind finds. With the ever-advancing social civilization, people gradually find coal hidden under the ground, so that the coal becomes one of important energy sources in the daily life of human beings. Later, people found petroleum resources, and the development and the use of the petroleum resources, wood, coal and other resources take a great step forward with the technological level. Although these energy sources are widely distributed and relatively widely used, they belong to non-renewable energy sources, and the continuous exploitation of human beings causes the shortage of required energy sources, which brings great challenges to the lives of people. Therefore, the search for sustainable renewable energy sources is urgent. The charge transfer of the supercapacitor is limited only at the electrolyte/electrode interface and no ionic diffusion occurs within the electrode material. A large amount of charge can be stored and discharged in a short time, resulting in a high power density. The super capacitor has attracted people's attention because of its simple principle, fast charge and discharge, long cycle life, high power density and low interface resistance. Supercapacitors can be divided into two categories: electric double layer capacitors and pseudocapacitors. Electric double layer capacitors store electrical energy by electrostatic accumulation of charge in the electric double layer at the electrode and electrolyte interfaces. The energy storage mechanism of the pseudocapacitor is the transfer process of surface Faraday electrons to metal ions, and can be realized by ion embedding or ion extraction. But generally lower energy densities limit their practical applications. Super capacitors are a new type of energy storage device that has the high energy density and long cycle life of conventional batteries. The secondary battery has high energy density (30-200Wh kg)-1) But with a lower power density (<1kW kg-1) (ii) a And the phase change generated in the charging and discharging process usually causes the electrode structure to change, thereby leading to lower power density (1 Wh kg)-1) And shorter cycle life. The super capacitor has the characteristics of high energy density, high charging and discharging speed, high safety, wide working temperature range and the like, and has become the firstOne of the scene energy storage devices. However, its lower energy density limits its further practical application, and therefore, how to increase the energy density of the supercapacitor becomes very important. Among the electrode materials, transition metal sulfide is a p-type semiconductor material having a narrow band gap with a band gap width of 1.2 to 2.1 eV. It has good stability below 800 deg.C. The chemical property is very stable, and the electric conductivity is good and the oxidation-reduction reaction is abundant. This has various advantages, such as: high oxidation state structure, large theoretical specific capacitance, and the like, which all make Co9S8Can be used as a good choice for manufacturing the electrode material of the battery. At present, Co has been widely studied9S8The material and the heterostructure thereof are used as electrode materials and in supercapacitors. The morphology based on the electrode material has a very large impact on the electrochemical performance of the material. Generally, metal oxides have poor conductivity and cycling stability, and then metal sulfides tend to have conductivity 10 to 100 times higher than oxides, so that transition group metal sulfides have high specific capacitance and good cycling performance due to high conductivity. By rationally designing the electrode material with high conductivity and unique morphological characteristics, the structural characteristics of the electrode material can be well optimized to a great extent.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a high-performance electrode material with a nano sea urchin structure, and solves the problems of low energy density, poor cycle performance, poor conductivity and the like of the material.
The invention is realized in such a way that a preparation method of a high-performance electrode material with a nano sea urchin structure comprises the following steps:
1) foam nickel pretreatment: putting the foamed nickel into deionized water containing 60ml for ultrasonic treatment for half an hour, then performing ultrasonic treatment for half an hour by using alcohol, and finally putting the foamed nickel into a vacuum drying oven to dry for 12 hours at the temperature of 60 ℃;
2) dissolving 2-6mmol of cobalt nitrate hexahydrate, 0.5-1.5g of ammonium fluoride and 0.5-2.0g of urea into 40-80ml of water, magnetically stirring for 20-45min, transferring the solution into a reaction kettle, preserving heat for 6-8h at the temperature of 100 ℃ and 120 ℃, naturally cooling to room temperature, and cleaning for 3-5 times by using absolute ethyl alcohol and deionized water to obtain a precursor;
3) adding 8-9mmol of sodium sulfide into 50-60ml of deionized water, magnetically stirring for 45min, transferring the precursor prepared in the step 2) into the reaction kettle, transferring the precursor into the reaction kettle, preserving heat for 4h at the temperature of 120 ℃ of 100-.
Further, the size of the foamed nickel is 3-5cm, and the foamed nickel is vertical to the bottom of the reaction kettle in the preparation process.
The chemical formula of the reaction is:
compared with the prior art, the invention has the beneficial effects that: the invention aims to synthesize a heterostructure with a unique structure by a simple hydrothermal method. The transition metal sulfide generally has a large number of reactive active sites, and meanwhile, the two-dimensional material also has high specific surface area, so that the two-dimensional material has stable structural characteristics in the electrochemical reaction process. Secondly, the nano sea urchin structure often shows good structural stability, and the obvious apical effect makes the nano sea urchin structure often show rich defect characteristics, which makes the electrode material have continuous active characteristics in the electrochemical reaction process. The invention aims to solve the technical problem of constructing a preparation method of a high-performance electrode material with a nano sea urchin structure. In addition, the method of directly growing on the current collector is adopted, so that the use of a conductive agent and a bonding agent can be effectively avoided. Meanwhile, the structure of the material is easily collapsed due to the presence of the conductive agent and the binder, resulting in poor electrochemical performance.
The invention discloses a preparation method of a high-performance electrode material with a nano sea urchin structure, which is Co directly grown on a foamed nickel current collector9S8An electrode material. The prepared electrode material is a high-performance electrode material self-assembled by nano sea urchins. The scanning electron microscope can find that the prepared electrode material is in a nano sea urchin structure with self-assembled nano wires and has stable structural characteristics. The beneficial electrolyte ions can be well transferred between the electrode material and the electrolyte. Meanwhile, the nanowire electrode material generally has a tip effect, which can accelerate charge transfer and is also beneficial to release of active sites, so that a good transfer channel can be provided for the transfer of electrons. In conclusion, various conditions enable the prepared electrode material to have good structural stability, and the structural stability can enable the electrode material to have good cycling stability. When the prepared electrode material is used as an electrode material, it exhibits a high mass specific capacitance of 1024Fg-1Meanwhile, as the current density is increased, the shape of the curve can be well maintained, which shows that the current-controlled linear motor has good rate performance.
Drawings
FIG. 1 is an X-ray diffraction pattern of the nano sea urchin structure of the present invention;
FIG. 2 is a scanning electron microscope of the nano-sea urchin structure of the present invention;
FIG. 3 is a scanning electron microscope of the nano-sea urchin structure of the present invention;
FIG. 4 is a cyclic voltammetry test of the nano sea urchin structure of the present invention;
FIG. 5 is a test of the charge and discharge of the nano sea urchin structure of the present invention;
FIG. 6 shows the cycle performance test of the nano sea urchin structure of the present invention;
FIG. 7 shows the cycle performance test of the nano sea urchin structure according to the present invention;
FIG. 8 shows the charge/discharge performance test of the nano sea urchin structure of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A preparation method of a high-performance electrode material with a nano sea urchin structure comprises the following steps; the medicines selected in the whole experimental process are analytically pure, and the purity of the medicines is 99.99%.
The size of the used nickel foam is 4cmx4cm, and the nickel foam can be ensured to be vertical to the bottom of the reaction kettle in the preparation process.
1) Dissolving 3mmol of cobalt nitrate hexahydrate, 1.0g of ammonium fluoride and 1.5g of urea in 40-80ml of water, stirring, reacting, cooling, cleaning and drying to obtain a prepared sample, magnetically stirring for 20-45min, transferring the prepared sample into the solution, transferring the solution into a reaction kettle, preserving heat at the temperature of 100-120 ℃ for 6h, naturally cooling to room temperature, and cleaning for 3 times by using absolute ethyl alcohol and deionized water to obtain a precursor.
2) Dissolving 6mmol of sodium sulfide in 50mL of deionized water, magnetically stirring for 45min, transferring the precursor prepared in the previous step into 40mL of deionized water, transferring the precursor into a reaction kettle, preserving heat for 4h at the temperature of 100-120 ℃, naturally cooling to room temperature, washing for 3-5 times by using absolute ethyl alcohol and deionized water, preserving heat for 12h at the temperature of 60 ℃ and drying the sulfide sample obtained in the step.
The reaction process is as follows:
example 2
Different from example 1, step 2)3mmol of cobalt chloride, 1.5g of urea, 0.9g of ammonium fluoride were dissolved in 40ml of water and stirred for 30 minutes; then transferring the solution into a reaction kettle, and preserving heat for 8 hours at 100 ℃; naturally cooling to room temperature, washing with anhydrous ethanol and deionized water for 3-6 times, and drying the prepared sample at 60 deg.C for 12 h;
3) dissolving 9g of sodium sulfide in 50ml of deionized water, magnetically stirring for 45min, transferring the prepared sample into the solution, transferring the solution into a reaction kettle, preserving heat for 4h at 120 ℃, naturally cooling to room temperature, washing for 3-5 times by using absolute ethyl alcohol and deionized water, preserving heat for 12h at 60 ℃ of the prepared sample, and drying.
The vulcanization will be omitted as a comparative experiment:
1) firstly, pretreating foamed nickel, putting a clean piece of foamed nickel into deionized water, carrying out ultrasonic treatment for half an hour, then carrying out ultrasonic treatment for 10 minutes by using alcohol, repeating the ultrasonic treatment for three times, and finally putting the foamed nickel into a vacuum drying oven for drying. Thus, organic impurities on the surface of the nickel oxide can be removed. Pretreating foamed nickel, performing ultrasonic treatment in deionized water for half an hour, performing ultrasonic treatment with alcohol for half an hour, and finally putting the foamed nickel into a vacuum drying oven for drying;
2) dissolving 2mmol of cobalt chloride, 1.0g of urea and 0.6g of ammonium fluoride in 40ml of water, and stirring for 30 minutes; then transferring the solution into a reaction kettle, and preserving heat for 8 hours at 100 ℃; naturally cooling to room temperature, washing with anhydrous ethanol and deionized water for 3-6 times, and drying the prepared sample at 60 deg.C for 12 h; the prepared sample has low specific capacitance as shown by electrochemical tests (see fig. 7 and 8).
The X-ray detection of the finished product obtained in example 1 showed that the diffraction peak energy was Co-localized as shown in FIG. 19S8Diffraction peak of (2) indicating echinoid Co9S8Nanowires were successfully prepared.
Referring to fig. 2 and 3, scanning electron microscope images of the prepared heterostructure electrode material show that the sample is a nano sea urchin structure with self-assembled nano-wires;
referring to fig. 4, in order to prepare cyclic voltammetry curve of the nano sea urchin electrode material, it can be found that the curve area is gradually increased along with the increase of the sweep rate.
As shown in FIG. 5, the discharge capacity of the prepared electrode material reaches 1024Fg-1And the specific capacitance is not reduced by times with the increase of the current density, which shows that the prepared electrode material has excellent rate performance.
See fig. 6, and the capacity retention after 10000 charge-discharge cycles was 85% (see fig. 5 charge-discharge test).
Referring to FIG. 7, the charge-discharge curve of the prepared comparative experimental electrode material can be found to reach 400Cg capacity-1The values are significantly lower than for the heterostructure after sulfurization.
Fig. 8 is a scanning electron microscope image of the heterostructure prepared without sulfidation, which shows that the material has non-uniform morphology and a certain amount of agglomeration, which is mainly caused by poor conductivity of the electrode material surface, and is easy to agglomerate.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (4)
1. A preparation method of a high-performance electrode material with a nano sea urchin structure is characterized by comprising the following steps:
1) foam nickel pretreatment: putting the foamed nickel into deionized water containing 60ml for ultrasonic treatment for half an hour, then performing ultrasonic treatment for half an hour by using alcohol, and finally putting the foamed nickel into a vacuum drying oven to dry for 12 hours at the temperature of 60 ℃;
2) dissolving 2-6mmol of cobalt nitrate hexahydrate, 0.5-1.5g of ammonium fluoride and 0.5-2.0g of urea into 40-80ml of water, magnetically stirring for 20-45min, transferring the solution into a reaction kettle, preserving heat for 6-8h at the temperature of 100 ℃ and 120 ℃, naturally cooling to room temperature, and cleaning for 3-5 times by using absolute ethyl alcohol and deionized water to obtain a precursor;
3) adding 6-9mmol of sodium sulfide into 50-60ml of deionized water, magnetically stirring for 45min, transferring the precursor prepared in the step 2) into the reaction kettle, transferring the precursor into the reaction kettle, preserving heat for 4h at the temperature of 120 ℃ of 100-.
2. The method of claim 1, wherein the nickel foam has a size of 3 to 5cm and is formed to be perpendicular to the bottom of the reaction vessel during the preparation process.
3. The method according to claim 1, wherein in step 2), 2mmol of cobalt nitrate hexahydrate, 0.8g of ammonium fluoride and 1.5g of urea are dissolved in 40ml of water, stirred for 20 minutes, then transferred to an 80ml reaction kettle and kept at 120 ℃ for 8 hours; naturally cooling to room temperature, and washing with anhydrous ethanol and deionized water for 5 times.
4. The method as claimed in claim 1, wherein in step 3), 8mmol of sodium sulfide is dissolved in 50ml of deionized water, magnetic stirring is carried out for 45min, then the precursor prepared in step 2) is transferred into the solution, and is transferred into a reaction kettle together, and is transferred into a 100ml reaction kettle, and the solution is kept warm for 4h at 120 ℃, and is cleaned by absolute ethyl alcohol and deionized water after being naturally cooled to room temperature.
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| US20170084924A1 (en) * | 2015-09-23 | 2017-03-23 | University Of Virginia Patent Foundation | Process of forming electrodes and products thereof from biomass |
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Application publication date: 20220415 |