CN110415985B - Positive active material, preparation method thereof, positive plate and super capacitor - Google Patents

Positive active material, preparation method thereof, positive plate and super capacitor Download PDF

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CN110415985B
CN110415985B CN201910559847.6A CN201910559847A CN110415985B CN 110415985 B CN110415985 B CN 110415985B CN 201910559847 A CN201910559847 A CN 201910559847A CN 110415985 B CN110415985 B CN 110415985B
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active material
lanio
positive electrode
nitrate hexahydrate
positive
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CN110415985A (en
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刘毅辉
何云斐
杨胜兵
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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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
    • H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • 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
    • 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
    • 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

Abstract

The invention relates to a super capacitorThe technical field, in particular to an anode active material, a preparation method thereof, an anode plate and a super capacitor, wherein the anode active material is LaNiO with nano-rod-shaped crystal grains3. The anode active material of the invention is LaNiO with nano-rod-shaped crystal grains3The material has the advantages of large specific surface area, stable structure, excellent conductivity, excellent cycling stability, higher specific capacity, better electrochemical stability and excellent super capacitor material; due to the change of the appearance, the specific capacitance, the internal resistance and the cycling stability of the super capacitor are obviously improved when the super capacitor is applied.

Description

Positive active material, preparation method thereof, positive plate and super capacitor
Technical Field
The invention relates to the technical field of super capacitors, in particular to a pole active material, a preparation method thereof, a positive plate and a super capacitor.
Background
With the rapid development of economy, the demand of socioeconomic energy sources is increasing year by year. The traditional energy sources mainly depend on fossil fuels such as coal, petroleum, natural gas and the like, but the reserves of the fossil fuels are limited, and resources are increasingly exhausted due to long-term over-exploitation; and fossil fuels release a large amount of greenhouse gases and harmful gases when being burned, which cause a series of environmental problems and also harm human health. Therefore, there is a need for more new energy sources that are clean and renewable to meet the needs of social development.
A super capacitor refers to a novel energy storage device between a traditional capacitor and a storage battery. The super capacitor has a higher energy density than a conventional capacitor, and at the same time, has a higher power density than various secondary batteries. At present, super capacitors are widely concerned by people due to the advantages of energy density close to batteries, high safety, environmental friendliness and the like. Therefore, the basic theory and practical application research of the super capacitor are deeply developed, and the method has important academic value and wide application prospect, and has important practical significance for solving the energy problem.
However, for supercapacitors, large-scale applications require challenges in terms of specific capacity and performance retention. In order to reduce the cost, improve the specific capacity and improve the performance retention rate, an effective method is to find a new electrode material or improve the performance of the existing material. The perovskite material has excellent performance, good conductivity, complex structure and stable chemical performance, so that the perovskite material has good electrochemical performance and is suitable for being used on a super capacitor with the cycle life reaching tens of thousands of times. However, the existing perovskite material lanthanum nickelate is mainly in the form of nano particles, nano hollow spheres and nano tubes, and the preparation process of the perovskite material lanthanum nickelate serving as the positive active substance of the super capacitor is complex.
Disclosure of Invention
One of the objects of the present invention is to provide a positive electrode active material, which is a nano-rod-shaped LaNiO3Large specific surface area, stable structure and excellent conductivity.
The second purpose of the invention is to provide a preparation method of the anode active material, the synthesis method is simple, alcohol organic matter is used as an additive, the appearance of the product crystal is improved, and the nano-rod-shaped LaNiO is obtained3。
The invention also aims to provide the positive plate which has high specific capacitance, small internal resistance of the electrode, good cycling stability and high charging and discharging efficiency.
The fourth purpose of the invention is to provide a super capacitor, which has fast charge and discharge speed, high efficiency and long cycle service life; the power density is high; the working temperature range is wide; maintenance is free; and the large-current discharge damage is small.
The scheme adopted by the invention for realizing one of the purposes is as follows: the positive active material is LaNiO with crystal grains in a nano rod shape3。
The second scheme adopted by the invention for achieving the purpose is as follows: a method for preparing a positive electrode active material, comprising the steps of:
a1, preparing a certain amount of lanthanum nitrate hexahydrate and nickel nitrate hexahydrate into a mixed solution with a certain concentration as a precursor solution;
a2, stirring the precursor solution obtained in the step A1 at normal temperature, adding an alkaline agent to adjust the pH of the solution during stirring, and stirring until a uniformly dispersed suspension is formed;
a3, adding a certain amount of alcohol organic matters into the suspension obtained in the step A2 to serve as a soft template, continuously stirring the mixture until the mixture is uniform, and then carrying out hydrothermal reaction at a certain temperature;
a4, centrifugally washing a precipitate obtained after the reaction in the step A3, and calcining the precipitate at a certain temperature to form a phase to obtain the anode active material LaNiO3。
Preferably, in the step A1, the molar ratio of lanthanum nitrate hexahydrate and nickel nitrate hexahydrate is 1:1, and the concentrations of lanthanum nitrate hexahydrate and nickel nitrate hexahydrate are both 0.02-0.04 mol/L.
Preferably, in the step a2, the alkaline agent is a KOH solution or a NaOH solution with a concentration of 6M, and is adjusted to pH 13.
Preferably, in the step a3, the volume ratio of the soft template to the precursor liquid is 6-11:1, and the soft template is polyethylene glycol.
The soft template is any one of polyethylene glycol 400, polyethylene glycol 12000, polyethylene glycol 6000 and polyethylene glycol 2000, preferably polyethylene glycol 400.
Preferably, in the step A3, the temperature of the hydrothermal reaction is 200-220 ℃.
Preferably, in the step A4, the calcination temperature is 700-3The crystal grains of (2) are in a nano rod shape.
The scheme adopted by the invention for realizing the third purpose is as follows: a positive plate comprises a plate substrate and a positive plate base, wherein the plate substrate comprises the following components in a mass ratio of 8:1:1 live LaNiO attached to the surface of the pole piece substrate3Acetylene black and polyvinylidene fluoride, wherein the LaNiO3Is the LaNiO3。
The scheme adopted by the fourth invention for realizing the purpose is as follows: a super capacitor adopts a positive active material comprising the LaNiO3。
The anode active material of the invention is LaNiO with nano-rod-shaped crystal grains3The material has the advantages of large specific surface area, stable structure, excellent conductivity, excellent cycling stability, higher specific capacity, better electrochemical stability and excellent super capacitor material; due to the change of the appearance, the method is applied to the super capacitor and found outThe specific capacitance, the internal resistance and the cycling stability are all obviously improved.
The preparation method of the anode active material takes the alcohol organic matter as the additive to achieve the aim of improving the crystal morphology and obtain the LaNiO with the nanorod structure3The material is prepared by firstly synthesizing the nanorod-structured LaNiO with large specific surface area, stable structure, excellent conductivity and excellent cycling stability by a soft template hydrothermal method3(ii) a Can effectively improve LaNiO3The electrochemical performance and the preparation method are simple.
The anode plate adopts nano rod-shaped LaNiO3As an active substance, the specific capacitance is obviously improved, the internal resistance of the electrode is reduced to some extent, the cycling stability is enhanced, and the charging and discharging efficiency in the cycling process is improved.
The super capacitor adopts nano rod-shaped LaNiO3As an active material, the charge-discharge speed is high, and the efficiency is high; the cycle service life is long; the power density is high; the working temperature range is wide; maintenance is free; and the large-current discharge damage is small.
Drawings
FIG. 1 shows LaNiO obtained in example 1 of the present invention3An XRD pattern of (a);
FIG. 2 shows LaNiO obtained in example 1 of the present invention3Scanning electron microscope images of;
FIG. 3 is an AC impedance spectrum of the positive electrode sheet obtained in example 2 of the present invention;
FIG. 4 is a cycle stability curve of the positive electrode sheet obtained in example 2 of the present invention;
FIG. 5 shows LaNiO obtained in comparative example 1 of the present invention3An XRD pattern of (a);
FIG. 6 shows LaNiO obtained in comparative example 1 of the present invention3Scanning electron microscope images of;
FIG. 7 is an AC impedance spectrum of a positive electrode sheet obtained in comparative example 2 of the present invention;
fig. 8 is a cycle stability curve of the positive electrode sheet obtained in comparative example 2 of the present invention.
Detailed Description
The following examples are provided to further illustrate the present invention for better understanding, but the present invention is not limited to the following examples.
In the following examples and comparative examples, the main apparatus and equipment were:
CS-150 electrochemical workstation; 101-O electric heating air blast drying box; JY202 precision electronic balance; 410HT numerical control ultrasonic cleaning instrument; MF-1100C medium temperature muffle furnace.
In the following examples and comparative examples, the main reagents were:
lanthanum nitrate hexahydrate (analytically pure); nickel nitrate hexahydrate (analytically pure); KOH (analytical grade); polyethylene glycol (analytical grade); n-methyl pyrrolidone (analytical grade); polyvinylidene fluoride (commercial grade); nickel foam (commercial grade).
In the following examples and comparative examples, the washing of the precipitate comprises the following steps:
(1) pouring the supernatant in the hydrothermal kettle, and pouring the lower-layer precipitate and liquid into a centrifugal tube;
(2) adding deionized water into a centrifugal tube, and then placing the centrifugal tube into a centrifugal machine for centrifugation;
(3) after centrifugation, pouring the liquid in the centrifugal tube, adding ethanol, and then putting the centrifugal tube into a centrifuge for centrifugation;
(4) after centrifugation, pouring out the liquid in the centrifugal tube, adding deionized water, and then placing the centrifugal tube into a centrifuge for centrifugation;
(5) after centrifugation, the liquid in the centrifuge tube was decanted off and the precipitate was dried in an oven.
In the following examples and comparative examples, the treatment of the nickel foam used comprises the following steps:
(1) cutting the foamed nickel into electrode slices of 1cm multiplied by 1cm, and respectively ultrasonically cleaning the electrode slices for 30 minutes by using acetone, ethanol and deionized water;
(2) drying in an oven at 80 deg.C for 8 hr.
In the following examples and comparative examples, electrochemical tests were conducted using a three-electrode system with a platinum wire electrode as the counter electrode and a mercury oxide electrode as the reference electrode.
Example 1
A positive electrode active material is prepared by the following steps:
0.87g of lanthanum nitrate hexahydrate and 0.58g of nickel nitrate hexahydrate are dissolved in 60ml of deionized water, the solution is stirred uniformly at room temperature by a magnetic stirrer, KOH is added to adjust the pH value to 13, and 10ml of polyethylene glycol (PEG-400) is added. And continuously stirring for 20 minutes to obtain a suspension, pouring the suspension into a hydrothermal kettle, and heating in an oven to obtain a precipitate. Washing and drying the precipitate, calcining in a medium-temperature muffle furnace at 750 deg.C for 3 hr to obtain powder, i.e. nano-rod-shaped LaNiO3。
As can be seen from FIG. 1, only LaNiO is present in the drawing3The characteristic diffraction peak of (A) does not have other miscellaneous peaks, which indicates that the pure-phase LaNiO is successfully prepared3。
From FIG. 2, LaNiO is clearly shown3The shape of the nano-rod is nano-rod, the size of the particle size is about 100nm in width and about 500nm in length.
Example 2
A positive plate is prepared by the following steps:
the nanorod-shaped LaNiO obtained in example 1 was added3Mixing the powder with acetylene black and polyvinylidene fluoride according to a mass ratio of 8:1:1, grinding for 30 minutes by using a mortar in a manual grinding mode to uniformly mix the powder, adding N-methyl pyrrolidone, performing ultrasonic uniform dripping on a pole piece substrate, putting the prepared electrode piece into an oven, heating to 80 ℃, keeping for 8 hours, drying and tabletting to obtain the positive pole piece.
FIG. 3 is the EIS curve of the positive plate of this example, the frequency range adopted by the electrochemical impedance test is 0.01Hz to 100000Hz, the scanning rate is 10mV/s, and it can be seen from FIG. 3 that the nano rod-shaped LaNiO is adopted3The internal resistance of the positive electrode sheet test as the positive electrode active material was 0.6125 Ω.
FIG. 4 is a cycle stability curve of the positive electrode sheet of this example, and it can be seen from FIG. 4 that the nano rod-shaped LaNiO is used3The initial specific capacitance of the positive plate test as the positive active material is 468.8F/g, the peak specific capacitance is 561.1F/g, and the charge-discharge efficiency after 2000 cycles is 98%.
Comparative example 1
A positive electrode active material is prepared by the following steps:
0.87g of lanthanum nitrate hexahydrate and 0.58g of nickel nitrate hexahydrate are dissolved in 70ml of deionized water, and the solution is stirred uniformly at room temperature by a magnetic stirrer, and KOH is added to adjust the pH value to 13. And continuously stirring for 20 minutes to obtain a suspension, pouring the suspension into a hydrothermal kettle, and heating in an oven to obtain a precipitate. Washing and drying the precipitate, calcining in a medium-temperature muffle furnace at 750 deg.C for 3 hr to obtain LaNiO powder3。
From FIG. 5, it can be seen that only LaNiO is present in the graph3The characteristic diffraction peak of (A) does not have other miscellaneous peaks, which indicates that the pure-phase LaNiO is successfully prepared3。
From FIG. 6, LaNiO can be seen3Is a nanoparticle with a particle size of greater than 100 nm.
Comparative example 2
A preparation method of a positive plate comprises the following steps:
LaNiO obtained in comparative example 1 was added3Mixing the powder with acetylene black and polyvinylidene fluoride according to a mass ratio of 8:1:1, grinding for 30 minutes by using a mortar in a manual grinding mode to uniformly mix the powder, adding N-methyl pyrrolidone, performing ultrasonic uniform dripping on a pole piece substrate, putting the prepared electrode piece into an oven, heating to 80 ℃, keeping for 8 hours, drying and tabletting to obtain the positive pole piece.
FIG. 7 is the EIS curve of the positive plate of this comparative example, the frequency range adopted by the electrochemical impedance test is 0.01Hz to 100000Hz, the scanning rate is 10mV/s, and it can be seen that the nano-particle LaNiO3The internal resistance of the positive electrode material of the supercapacitor is 2.277 omega.
FIG. 8 is a cycle stability curve of the positive electrode sheet of this comparative example, in which it can be seen that the nano-particle LaNiO3The initial specific capacitance of the capacitor is 299.2F/g, the peak specific capacitance of the capacitor is 299.2F/g, and the charge-discharge efficiency after 2000 cycles is 81 percent.
As can be seen from examples 1-2 and comparative examples 1-2, LaNiO prepared by the present invention3The crystal grain of the invention is a special structure of a nano rod, and the test result shows that the nano rod-shaped LaNiO of the invention3The material has excellent electricityChemical properties, specific capacitance and internal resistance of the nano-particle structure are far lower than those of common LaNiO with a nano-particle structure3Material, so the LaNiO of nanorod structure3The material has great potential in the aspect of energy storage of the super capacitor.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.

Claims (7)

1. A method for preparing a positive electrode active material, characterized in that: the positive active material is LaNiO with nano-rod-shaped crystal grains3；
The preparation method of the positive active material comprises the following steps:
a1, preparing a certain amount of lanthanum nitrate hexahydrate and nickel nitrate hexahydrate into a mixed solution with a certain concentration as a precursor solution;
a2, stirring the precursor solution obtained in the step A1 at normal temperature, adding an alkaline agent to adjust the pH of the solution during stirring, and stirring until a uniformly dispersed suspension is formed;
a3, adding a certain amount of alcohol organic matters into the suspension obtained in the step A2 to serve as a soft template, continuously stirring the mixture until the mixture is uniform, and then carrying out hydrothermal reaction at a certain temperature;
a4, centrifugally washing a precipitate obtained after the reaction in the step A3, and calcining the precipitate at a certain temperature to form a phase to obtain the anode active material LaNiO3；
In the step A3, the volume ratio of the soft template to the precursor liquid is 6-11:1, and the soft template is polyethylene glycol.
2. The method for producing a positive electrode active material according to claim 1, characterized in that: in the step A1, the molar ratio of lanthanum nitrate hexahydrate to nickel nitrate hexahydrate is 1:1, and the concentrations of lanthanum nitrate hexahydrate and nickel nitrate hexahydrate are both 0.02-0.04 mol/L.
3. The method for producing a positive electrode active material according to claim 1, characterized in that: in the step A2, the alkali agent is 6M KOH solution or NaOH solution, and the pH is adjusted to 13.
4. The method for producing a positive electrode active material according to claim 1, characterized in that: in the step A3, the temperature of the hydrothermal reaction is 200-220 ℃.
5. The method for producing a positive electrode active material according to claim 1, characterized in that: in the step A4, the calcination temperature is 700-750 ℃, and the anode active material LaNiO is3The crystal grains of (2) are in a nano rod shape.
6. A positive electrode sheet characterized in that: the electrode plate comprises a pole piece substrate and a base material, wherein the pole piece substrate comprises the following components in percentage by mass 8:1:1 LaNiO attached to the surface of the pole piece substrate3Acetylene black and polyvinylidene fluoride; wherein, the LaNiO3LaNiO prepared by the preparation method of any one of claims 1 to 53。
7. A supercapacitor, characterized by: the positive active material adopted by the super capacitor comprises LaNiO prepared by the preparation method of any one of claims 1 to 53。
CN201910559847.6A 2019-06-26 2019-06-26 Positive active material, preparation method thereof, positive plate and super capacitor Active CN110415985B (en)

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* Cited by examiner, † Cited by third party
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US9607764B2 (en) * 2010-10-20 2017-03-28 Chun-Yen Chang Method of fabricating high energy density and low leakage electronic devices
CN103021678A (en) * 2013-01-22 2013-04-03 电子科技大学 Preparation of super capacitor film electrode capable of charging and discharging at ultra-high rate
JP6024502B2 (en) * 2013-02-13 2016-11-16 三菱マテリアル株式会社 Composition for forming LaNiO3 thin film and method for forming LaNiO3 thin film using this composition
JP6365294B2 (en) * 2014-03-25 2018-08-01 三菱マテリアル株式会社 Method for forming LaNiO3 thin film
CN105170050B (en) * 2015-09-16 2017-03-22 齐齐哈尔大学 Preparation method of LaNiO3 ball with micro-nano structure
CN105609325B (en) * 2016-03-11 2018-02-27 天津大学 A kind of LaNiO with hollow structure3Sub-meter grade microballoon electrode material preparation method
CN107119305A (en) * 2017-05-03 2017-09-01 厦门大学 The preparation method of the nano-particle modified Nano tube array of titanium dioxide of nickel acid lanthanum
CN109326778B (en) * 2018-09-11 2021-08-24 武汉理工大学 Lanthanum nickelate coated ternary cathode material and preparation method thereof
CN109671566A (en) * 2018-11-30 2019-04-23 歌尔股份有限公司 A kind of preparation method and multilayer electronic device of multilayer electronic device

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