CN111899988A - Macro preparation method and application of nickel-cobalt double-metal hydroxide electrode material - Google Patents
Macro preparation method and application of nickel-cobalt double-metal hydroxide electrode material Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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Abstract
The invention discloses a macroscopic preparation method and application of a nickel-cobalt double metal hydroxide electrode material. Adjusting the pH value of the mixed solution by dropwise adding ammonia water; and finally, placing the obtained suspension in an oil bath kettle for further heating and stirring to fully react, removing redundant impurities through centrifugal washing, and drying to obtain the nickel-cobalt double hydroxide. The method has the advantages of simple process, low cost and the like, and particularly, the method obtains the required product by a chemical coprecipitation method, has mild and controllable reaction conditions, and is easy to realize the large-scale production of the nano electrode material. The invention provides a universal synthetic route for efficiently preparing high-performance electrode materials, and the prepared nickel-cobalt double metal hydroxide shows high specific capacity, good rate performance and cycling stability when being used as a super capacitor electrode material.
Description
Technical Field
The invention belongs to the field of electrochemical energy storage, and particularly relates to a macroscopic preparation method and application of a nickel-cobalt double-metal hydroxide electrode material.
Background
As a novel energy storage device, the super capacitor has multiple advantages of high power density, quick charge and discharge, long service life and the like. However, the energy density of supercapacitors is lower compared to batteries. The energy density of the super capacitor can be improved by improving the electrochemical performance of the electrode material. The layered transition metal hydroxide has the advantages of high theoretical specific capacity, lower cost, environmental friendliness and the like, and is considered to be one of the most potential electrode materials. The nickel-cobalt layered double hydroxide has important significance in realizing high specific capacity of the electrode material, improving rate capability and the like due to the synergistic effect between Ni and Co elements and abundant electroactive sites caused by various redox states.
At present, the methods for synthesizing nickel-cobalt double metal hydroxide with a nano structure and capable of realizing good energy storage performance mainly comprise a hydrothermal method, a template method, a conductive substrate in-situ growth method, electrochemical deposition and the like. The nickel-cobalt layered double-metal hydroxide electrode material obtained by part of the synthesis method has excellent electrochemical performance, but the preparation process is complex, the repeatability is poor and the cost is high; part of the synthesis methods have simple preparation processes, but the capacitance performance of the product is poor. Based on this, how to further simplify the preparation process, realize higher yield, and ensure the excellent electrochemical properties (high specific capacitance, good rate performance and cycle stability) of the nickel-cobalt double hydroxide is crucial to the industrial production of the nickel-cobalt double hydroxide.
The subject group of the professor Wuli Min of the university of Compound denier (adv. Funct. Mater.2014,24,934-942) adopts a hydrothermal method (under the reaction conditions of 180 ℃ and 24 hours) to grow nickel-cobalt layered hydroxide on the foamed nickel in situ, and the composite electrode is arranged at 3A g-1At current density, the ultra-high specific capacitance (2682F g) is displayed-1)。However, the method is not suitable for mass production due to the limitations of reaction conditions and yield.
The project group (adv. Funct. Mater.2018,1803272) of Qiu Jie mountain professor of Beijing university of chemical industry synthesizes nickel-cobalt layered hydroxide ultrathin nanosheets through graphene oxide surface confinement induction, and a product is obtained after treatment for 5 hours in an oil bath kettle at 95 ℃, and when the product is used as an electrode material of a super capacitor, the super capacitor has higher charge storage capacity, and the specific capacitance of the super capacitor is up to 1489F g-1Good cycle performance (at 6 Ag)-1Capacity retention was 80% after 5000 cycles at current density). The Jae SuYu professor team of the university of Chongqing in Korea firstly chemically deposits Ni on polyester fabric, and then obtains the nickel-cobalt double-metal hydroxide flexible electrode material through chemical bath and electrochemical deposition, and the composite electrode is arranged at the electrode with the thickness of 2mA cm-2The maximum area capacity at current density was 536.96. mu. Ah cm-2. The nickel-cobalt double-metal hydroxide electrode material with excellent energy storage performance is prepared by the synthesis method or the strategy, but the synthesis process can be further simplified, so that the nickel-cobalt double-metal hydroxide electrode material can realize high yield under the condition of high efficiency and economy, and simultaneously ensures that the material has excellent electrochemical performance, and has high specific capacitance, power density and cycling stability when being used as a super capacitor electrode material.
Disclosure of Invention
The invention aims to provide a macroscopic preparation method and application of a nickel-cobalt double-metal hydroxide electrode material. The method is simple and controllable, and can realize large-scale preparation. Compared with the traditional hydrothermal method or electrochemical deposition method and the like, the method adopts a simple chemical coprecipitation method, provides an alkaline reaction environment by slowly regulating and controlling the pH of the mixed solution, and realizes (M)2++2OH-→M(OH)2And M ═ Ni and Co) under mild experimental conditions (50-70 ℃ under atmospheric pressure), a large yield can be achieved, and good electrochemical performance can be obtained.
The macroscopic preparation method of the nickel-cobalt double metal hydroxide electrode material comprises the following steps:
step 1: dissolving a nickel source and a cobalt source in a mixed solution of deionized water and ethanol according to a certain proportion, adding ammonium chloride after dissolution for regulating and controlling morphology and a precipitator urea, and stirring until dissolution.
Step 2: and (3) dropwise adding ammonia water into the system obtained in the step (1), adjusting the pH value to obtain a dark green suspension, and heating and stirring the obtained suspension to enable the reaction to be more uniform and sufficient.
And step 3: collecting the product nickel cobalt hydroxide obtained by the reaction, centrifugally washing to remove redundant impurities, and drying to obtain the final product.
In step 1, the nickel source is soluble nickel salt including Ni (NO)3)2And hydrates thereof, NiSO4And hydrates thereof, NiCl2And hydrates thereof; the cobalt source is a soluble cobalt salt comprising Co (NO)3)2And hydrates thereof, CoSO4And hydrates thereof, CoCl2And hydrates thereof.
In the step 1, the molar ratio of the nickel source to the cobalt source is 1: (0.2-5).
In the step 1, the volume ratio of water to ethanol in the mixed solvent is (4-1): 1.
in step 1, the ratio of the total molar amount of the nickel source and the cobalt source to the molar amount of the urea is 1: (4-6); the molar ratio of ammonium chloride to urea is 1: (2-5).
In the step 2, the concentration range of the ammonia water is 5-20 wt%; adjusting the pH value to 8.5-10.
In the step 2, the obtained suspension is heated to 50-70 ℃, and stirred to react for 8-12 hours.
And in the step 3, alternately washing for multiple times by adopting water and a mixed solution of ethanol and water, wherein the volume ratio of ethanol to water in the mixed solution of ethanol and water is (0.2-1): 1.
in the step 3, the drying temperature is 60 ℃ and the drying time is 12-20 h.
The nickel-cobalt double-metal hydroxide electrode material prepared by the method can be used as a super capacitor anode material and has good electrochemical performance.
The invention has the beneficial effects that:
(1) the method has the advantages of abundant raw materials, safety, no pollution, simple operation, low cost and high yield.
(2) The method has mild reaction conditions, does not need conditions such as high temperature, high pressure or external voltage, and the like, can realize the macroscopic preparation of the electrode material by enlarging a reaction vessel and increasing the consumption of raw materials, provides a universal synthetic route for efficiently preparing the high-performance supercapacitor anode material, and paves the way for the realization of the high-performance supercapacitor anode material.
(3) The obtained nickel-cobalt double metal hydroxide electrode material has a nano-flake structure, is beneficial to ion rapid transmission, and shows high specific capacitance, good rate performance and cycle life when being used as a super capacitor electrode material.
Drawings
FIG. 1 shows Ni obtained in example 12Co1SEM picture of-LDH and schematic representation of the synthesis reaction which can be carried out in a large-volume vessel.
FIG. 2 shows Ni obtained in example 12Co1Electrochemical performance of LDH in a three-electrode system: (a) a CV curve; (b) a CD curve; (c) specific capacities obtained at different current densities; (d) and (4) cycle performance.
FIG. 3 shows Ni obtained in example 21Co1SEM picture of-LDH.
FIG. 4 shows Ni obtained in example 21Co1Electrochemical performance of LDH in a three-electrode system: (a) a CV curve; (b) a CD curve; (c) specific capacities obtained at different current densities; (d) and (4) cycle performance.
Fig. 5 is the electrochemical performance of the hybrid supercapacitor assembled in example 2: (a) a CV curve; (b) a CD curve; (c) specific capacities were obtained at different current densities.
Detailed Description
The technical solution of the present invention is further illustrated by the following examples, which are provided to more clearly illustrate the performance of the present invention, but are not limited to the following examples.
Example 1:
40mmol of NiCl2·6H2O and 20mmol CoCl2·6H2Dissolving O in a mixed solution of 600mL of deionized water and 200mL of ethanol, stirring until the O is dissolved,6.4g of NH were then added4Cl and 14.4g of urea are stirred and dissolved; dropwise adding 10% ammonia water to adjust the pH value to 9, stopping adding the mixture into a 60 ℃ oil bath kettle, stirring for 10 hours, and naturally cooling; centrifugally washing with deionized water and ethanol for 4 times, collecting the product, and drying in an oven at 60 deg.C for 12 hr to obtain Ni2Co1-LDH。
This example uses a simple chemical coprecipitation method, the whole reaction process is carried out in a 1L glass bottle (FIG. 1), and Ni is obtained by adjusting and controlling a suitable pH value and a suitable reaction process2Co1LDH powder yield exceeding 1.5g, synthesized Ni2Co1The LDH is a flower-shaped structure composed of sheets, and the two-dimensional sheet structure has more active sites, can improve the kinetics of electrochemical reaction, and simultaneously provides a quick ion transmission path, thereby being beneficial to realizing better rate performance of an electrode material.
Ni obtained in the example2Co1The use of LDH as supercapacitor electrode material is as follows: assembling a three-electrode system using Ni2Co1LDH as an active material, conductive carbon black (SP) as a conductive agent, and polyvinylidene fluoride (PVDF) as a binder (mass ratio of 80: 10: 10) were coated on a base graphite paper (1 cm. times.2 cm) in an area of 1cm to prepare an electrode slurry2And drying the left and right parts to be used as working electrodes. Ag/AgCl as reference electrode, Pt counter electrode and Ni2Co1LDH was the working electrode, 1MKOH was the electrolyte, and the electrochemical performance of the electrode material in a three-electrode system was tested (FIG. 2). The Cyclic Voltammetry (CV) curves and constant current Charge and Discharge (CD) curves in FIG. 2 show the synthesized Ni2Co1The LDH shows the behavior of a typical battery type material, and the maximum specific capacitance reaches 685.8C g-1(1A g-1At current density) at 20A g-1The capacity retention rate was 82% at current density, indicating good rate performance. Ni obtained by this example2Co1LDH electrode materials at 10A g-1The electrode material is cycled for 5000 times under constant current charge and discharge, and the capacity is 85.2 percent of the initial capacity, which shows that the electrode material has better cycling stability.
Example 2:
20mmol of NiCl2·6H2O and 20mmol CoCl2·6H2O is dissolved in a mixed solution of 600mL of deionized water and 200mL of ethanol, stirred until dissolved, and then 4.3g of NH is added4Cl and 9.6g of urea are stirred until the Cl and the urea are dissolved; dropwise adding 5% ammonia water to adjust pH until pH is 9, placing into a 60 deg.C oil bath, and stirring for 10 hr; centrifugally washing with deionized water and ethanol for 4 times, collecting the product, and drying in an oven at 60 deg.C for 12 hr to obtain Ni1Co1-LDH。
Ni to be obtained1Co1LDH electrodes were prepared as in example 1, assembling a three-electrode test system. Ni1Co1The micro-morphology of the LDH is shown in figure 3 and is a flower-like morphology formed by ultrathin nanosheets. Ni1Co1The LDH electrodes exhibited better supercapacitive performance (FIG. 4) at current densities of 1, 2, 5, 10 and 20A g-1In time of (i), Ni1Co1The specific capacities of the LDH electrodes were 766, 743, 708, 679 and 642C g, respectively-1. The electrode has good rate capability (at 20A g)-1Capacity retention 84% at current density) and cycle life (at 10A g)-1The capacity retention rate is 87.4 percent after 5000 cycles under the current density, which shows that the energy storage performance of the electrode material can be further improved by regulating the proportion of nickel and cobalt.
To further increase the utility of the invention, we will use the Ni obtained in this example1Co1The electrochemical performance of a hybrid supercapacitor assembled with an LDH electrode as positive electrode, activated carbon as negative electrode, potassium hydroxide-doped polybenzimidazole as electrolyte and a separator, tested (fig. 5), and having a large specific capacitance (at 0.5A g)-1At current density, the specific capacitance is 161F g-1) The energy storage device has good application potential.
Claims (9)
1. A macroscopic preparation method of a nickel-cobalt double metal hydroxide electrode material is characterized by comprising the following steps:
step 1: dissolving a nickel source and a cobalt source in a mixed solution of deionized water and ethanol according to a certain proportion, adding ammonium chloride after dissolution for regulating and controlling morphology and a precipitator urea, and stirring until dissolution.
Step 2: and (3) dropwise adding ammonia water into the system obtained in the step (1), adjusting the pH value to obtain a dark green suspension, and heating and stirring the obtained suspension to enable the reaction to be more uniform and sufficient.
And step 3: collecting the product nickel cobalt hydroxide obtained by the reaction, centrifugally washing to remove redundant impurities, and drying to obtain the final product.
2. The method of claim 1, wherein:
in step 1, the nickel source is soluble nickel salt including Ni (NO)3)2And hydrates thereof, NiSO4And hydrates thereof, NiCl2And hydrates thereof; the cobalt source is a soluble cobalt salt comprising Co (NO)3)2And hydrates thereof, CoSO4And hydrates thereof, CoCl2And hydrates thereof.
3. The method of claim 2, wherein:
in the step 1, the molar ratio of the nickel source to the cobalt source is 1: (0.2-5).
4. The method of claim 1, wherein:
in the step 1, the volume ratio of water to ethanol in the mixed solvent is (4-1): 1.
5. the method of claim 1, wherein:
in step 1, the ratio of the total molar amount of the nickel source and the cobalt source to the molar amount of the urea is 1: (4-6); the molar ratio of ammonium chloride to urea is 1: (2-5).
6. The method of claim 1, wherein:
in the step 2, the concentration range of the ammonia water is 5-20 wt%; adjusting the pH value to 8.5-10.
7. The method of claim 1, wherein:
in the step 2, the obtained suspension is heated to 50-70 ℃, and stirred to react for 8-12 hours.
8. The method of claim 1, wherein:
and in the step 3, alternately washing for multiple times by adopting water and a mixed solution of ethanol and water, wherein the volume ratio of ethanol to water in the mixed solution of ethanol and water is (0.2-1): 1.
9. use of a nickel cobalt double hydroxide electrode material obtained by the preparation according to any one of the methods described in claims 1 to 8, characterized in that: the nickel-cobalt double metal hydroxide electrode material is used as a super capacitor positive electrode material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112877712A (en) * | 2021-01-13 | 2021-06-01 | 吉林大学 | Transition metal phosphorus sulfide and preparation method and application thereof |
| CN114335448A (en) * | 2022-01-04 | 2022-04-12 | 湖北大学 | Nickel-cobalt hydroxide with multilayer nanosheet structure and preparation method and application thereof |
| CN114715954A (en) * | 2022-03-21 | 2022-07-08 | 东北电力大学 | Preparation method and application of NiMn-LDH material after three-dimensional flower-ball-shaped partial vulcanization |
| CN114853092A (en) * | 2022-03-30 | 2022-08-05 | 武汉工程大学 | Preparation method of nano-scale double transition metal oxide with large specific surface area |
| CN114937769A (en) * | 2022-06-15 | 2022-08-23 | 格林美（无锡）能源材料有限公司 | Washing-free high-rate hollow high-nickel cathode material and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112877712A (en) * | 2021-01-13 | 2021-06-01 | 吉林大学 | Transition metal phosphorus sulfide and preparation method and application thereof |
| CN114335448A (en) * | 2022-01-04 | 2022-04-12 | 湖北大学 | Nickel-cobalt hydroxide with multilayer nanosheet structure and preparation method and application thereof |
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| CN114715954A (en) * | 2022-03-21 | 2022-07-08 | 东北电力大学 | Preparation method and application of NiMn-LDH material after three-dimensional flower-ball-shaped partial vulcanization |
| CN114715954B (en) * | 2022-03-21 | 2023-06-20 | 东北电力大学 | Preparation method and application of NiMn-LDH material after three-dimensional flower-sphere-shaped partial vulcanization |
| CN114853092A (en) * | 2022-03-30 | 2022-08-05 | 武汉工程大学 | Preparation method of nano-scale double transition metal oxide with large specific surface area |
| CN114937769A (en) * | 2022-06-15 | 2022-08-23 | 格林美（无锡）能源材料有限公司 | Washing-free high-rate hollow high-nickel cathode material and preparation method and application thereof |
| CN114937769B (en) * | 2022-06-15 | 2023-12-05 | 格林美（无锡）能源材料有限公司 | No-water-washing high-magnification hollow high-nickel cathode material and preparation method and application thereof |
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Application publication date: 20201106 |