CN101950680B - Nano nickel oxide composite electrode for super capacitor and preparation method thereof - Google Patents
Nano nickel oxide composite electrode for super capacitor and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a nano nickel oxide composite electrode for a super capacitor and a preparation method thereof. The preparation material of the electrode is a composite material prepared by adding a certain amount of metal elements into powdery nano nickel oxide material. The method comprises the following steps of: 1) preparing nickel salt aqueous solution in which a metal salt is added, and adding the metal elements; 2) preparing mixed solution A; 3) preparing mixed solution B; 4) mixing the mixed solution A and the mixed solution B; 5) performing solid-liquid separation on the slurry and drying the solid to obtain a calcination precursor; and 6), calcining the precursor to obtain the nano nickel oxide composite electrode, and preparing the electrode by a routine method in which the prepared material serves as an active substance. The method has the advantages that: the electrode has high specific capacity and strong large current discharging ability; the effective service life is prolonged; compared with the traditional technology, the method has the advantages of simplified technical process, stable process and easy operation; the quality of the product is safe and reliable; and the cost is low.
Description
Technical field
The present invention relates to a kind of nano nickel oxide composite electrode for ultracapacitor and preparation method thereof, belong to the electrode material preparing technical field.
Background technology
Ultracapacitor is a kind of novel energy-storing device between physics electric capacity and storage battery, have than the much higher energy density of traditional capacitor and the power density more much bigger than storage battery, integrate long, the characteristic such as power density is high, serviceability temperature wide ranges, charging rate are fast of life-span.These good characteristics of ultracapacitor have extremely widely it and use in the fields such as traffic, radio communication, military affairs, clean energy resource system.
As a kind of electrode material for ultracapacitor, nano-nickel oxide attracts tremendous attention because having the characteristics such as specific area height, serviceability temperature wide ranges, cost be low.
Be in the Chinese patent application of CN1887728A at publication number, reported that a kind of electrochemical capacitor is with the preparation method of nickel oxide.The method comes dispersing nanoparticles to obtain the nickel oxide electrode material of high-ratio surface by adding surfactant.But the intermediate products nickel hydroxide must be through cyclic washing to remove unnecessary surfactant, and technical process is loaded down with trivial details.The specific capacity of active material is only about 200 F/g in the nano nickel oxide electrode of the method preparation.
Be in the Chinese patent application of CN1944276A at publication number, disclose take nickel salt, ammoniacal liquor and NaOH as raw material that precipitation prepares the method for nano-nickel oxide by high-temperature calcination in alcohol solution.The method precipitation process is slow, and has equally also comprised interpolation and the washing process of surfactant, and the specific capacity of active material is less than 300 F/g in the nano nickel oxide electrode of preparation.
The specific capacity of the nano nickel oxide electrode material of prior art is generally on the low side, and the liquid phase preparation process of material is general consuming time longer, and has mostly used surfactant, makes aftertreatment technology loaded down with trivial details.In order to improve the specific capacity of nano nickel oxide electrode material, can in the nickel oxide lattice, mix metallic element formation nickel oxide combination electrode material.Be in the Chinese patent application of CN101333008A at publication number, a kind of preparation method of nanometer nickel oxide composite powder is disclosed, the nickel oxide combination electrode that the method makes, its active material comprises cobalt and two kinds of doping elements of zinc, specific capacity reaches 348～360F/g, and the purer nano nickel oxide electrode material of this numerical value increases, but since the single and total incorporation of doping element only between 1.1% to 20%, therefore, the Amplitude Ratio of specific capacity raising is more limited.In addition, the method also need add the multiple industrial chemicals that add such as acrylamide, lattice reagent, and preparation technology is loaded down with trivial details, cost is higher.
Summary of the invention
First purpose of the present invention is: overcome the defective that existing electrode of super capacitor exists, a kind of nano nickel oxide composite electrode for ultracapacitor is provided, it has height ratio capacity, strong large current discharging capability, and prolongs Acceptable life.
Second purpose of the present invention is: overcome the defective that existing super capacitor composite electrode preparation method exists, a kind of method for preparing composite electrode for ultracapacitor is provided, the relative prior art of the method, process simplification, process stabilizing, easy operating make Product quality and safety reliable and cost is low.
Realize that a kind of nano nickel oxide composite electrode technical scheme for ultracapacitor of the present invention is: it is to mix a certain amount of metallic element and the composite material made at Powdered nano oxidized nickel material that its system is joined material; Described metallic element is one or more combinations in cobalt, manganese, yttrium, lutetium, cadmium, the ytterbium.
Further technical scheme is:
Described nano nickel oxide composite electrode for ultracapacitor, in Powdered nano oxidized nickel material, mix a certain amount of metallic element, its metallic element incorporation is: the configuration nickel salt and mix in the mixed aqueous solution of slaine, the slaine total concentration is 0.01～1mol/L, and total mol ratio of wherein mixing metallic element and nickel element is 1:1～9.
Described nano nickel oxide composite electrode for ultracapacitor, its nickel salt are at least a material in Nickel dichloride hexahydrate, Nickelous nitrate hexahydrate, the six hydration nickel sulfate; The described slaine that mixes is selected from hydrochloride, nitrate, the sulfate one or more.
Described nano nickel oxide composite electrode for ultracapacitor, it mixes metallic element and is selected from cobalt, manganese, yttrium, lutetium, cadmium, the ytterbium two kinds.
Described nano nickel oxide composite electrode for ultracapacitor, it mixes metallic element and is selected from three kinds of combinations in cobalt, manganese, yttrium, lutetium, cadmium, the ytterbium.
Described nano nickel oxide composite electrode for ultracapacitor, it mixes metallic element is cobalt, manganese, yttrium, lutetium, cadmium, ytterbium.
Described nano nickel oxide composite electrode for ultracapacitor, it mixes metallic element and is selected from cobalt and manganese and yttrium and the cadmium one or more.
Realize the technical scheme of the nano nickel oxide composite electrode compounding method for ultracapacitor of the present invention, comprise following processing step:
1) configuration nickel salt and the aqueous solution that mixes slaine, the slaine total concentration is 0.01～1mol/L, total mol ratio of wherein mixing metallic element and nickel element is 1:1～9; The described metallic element that mixes is one or more combinations in cobalt, manganese, yttrium, lutetium, cadmium, the ytterbium;
2) adding volume in the above-mentioned aqueous solution is the organic solvent of 0.1～4 times of aqueous solvent volume, obtains mixed solution A;
3) aqueous solution of configuration carbonic hydroammonium, then adding volume is the organic solvent of 0.1～4 times of aqueous solvent volume, obtains mixed solution B, and wherein the concentration of carbonic hydroammonium is 0.01～1mol/L, and the kind of organic solvent is consistent with mixed solution A;
4) above-mentioned mixed solution A was stirred 10～60 minutes, add fast subsequently mixed solution B and stirring within 30～300 seconds time, the pH value of control solution is 7～9, and the reaction time was at 1～3 hour;
5) above-mentioned reaction is carried out Separation of Solid and Liquid to slurry after finishing, and precipitation is washed with water 2～5 times, in 50～150 ℃ of dryings 5～24 hours, obtains calcining precursor;
6) above-mentioned calcining precursor was calcined 2～6 hours under 250～450 ℃, namely made particle diameter at the nano nickel oxide composite electrode material of 30～50nm, make electrode take prepared material as active material with conventional method again.
Further technical scheme is:
The preparation method of described nano nickel oxide composite electrode for ultracapacitor, its organic solvent is one or more the mixing in alcohols and the organic solvent of ketone.
The preparation method of described nano nickel oxide composite electrode for ultracapacitor, its preparation process is:
1) configuration nickel salt and the aqueous solution that mixes slaine, the slaine total concentration is 0.01～1mol/L, total mol ratio of wherein mixing metallic element and nickel element is 1:9; The described metallic element that mixes is selected from cobalt, also can be a kind of in manganese, yttrium, lutetium, cadmium, the ytterbium;
2) adding volume in the above-mentioned aqueous solution is the absolute ethyl alcohol of 0.1～4 times of aqueous solvent volume, obtains disposing the alcohol of slaine-water mixed solution A;
3) aqueous solution of configuration carbonic hydroammonium, then adding volume is the absolute ethyl alcohol of 0.1～4 times of aqueous solvent volume, obtains mixed solution B, wherein the concentration of carbonic hydroammonium is 0.01～1mol/L;
4) above-mentioned mixed solution A was stirred 30 minutes, within 30～300 seconds time, add fast subsequently above-mentioned ammonium bicarbonate soln, i.e. mixed solution B and stirring, the pH value of control solution is 7～9, and the reaction time was at 1～3 hour;
5) above-mentioned reaction is carried out Separation of Solid and Liquid to slurry after finishing, and precipitation is washed with water 2～5 times, in 100 ℃ of dryings 12 hours, obtains calcining precursor;
6) above-mentioned calcining precursor was calcined 3 hours under 350 ℃, namely made particle diameter at the nano nickel oxide composite electrode material of 30～45nm, make electrode take prepared material as active material with conventional method again.
Remarkable beneficial effect of the present invention is:
1, mixing of a large amount of metallic elements makes that the specific capacity of active material significantly promotes in the nickel oxide electrode, reaches as high as more than the 1000F/g, and simultaneously, this nickel oxide combination electrode also has stronger large current discharging capability;
2, the nickel oxide combination electrode material epigranular that makes, particle diameter are between 30～50nm, and dispersiveness better; 3, adopt the method for rapid precipitation, shortened the liquid phase reactor time, and do not used surfactant, simplified aftertreatment technology, therefore, whole preparation process shortens relatively, and technological parameter is controlled easily.
Embodiment
Be described further as follows to this bright a kind of nano nickel oxide composite electrode for ultracapacitor in conjunction with the embodiments:
Embodiment 1:It is to mix a certain amount of metallic element and the composite material made in Powdered nano oxidized nickel material that a kind of nano nickel oxide composite electrode for ultracapacitor, its system are joined material; Described metallic element is one or more combinations in cobalt, manganese, yttrium, lutetium, cadmium, the ytterbium.Describedly in Powdered nano oxidized nickel material, mix a certain amount of metallic element, its metallic element incorporation is: the configuration nickel salt and mix in the mixed aqueous solution of slaine, the slaine total concentration is 0.01～1mol/L, total mol ratio of wherein mixing metallic element and nickel element is 1:1～9, and the total mol ratio of present embodiment is 1:2; Described nickel salt is at least a material in Nickel dichloride hexahydrate, Nickelous nitrate hexahydrate, the six hydration nickel sulfate, and present embodiment is two kinds of Nickel dichloride hexahydrate, Nickelous nitrate hexahydrates; The described slaine that mixes is selected from hydrochloride, nitrate, the sulfate one or more, and present embodiment is two kinds in hydrochloride, nitrate; The described metallic element that mixes is selected from cobalt, manganese, yttrium, lutetium, cadmium, the ytterbium two kinds, and the particle diameter of this combination electrode material is 40～50nm.
Embodiment 2:As different from Example 1, the configuration nickel salt and mix in the mixed aqueous solution of slaine, total mol ratio of mixing metallic element and nickel element is 1:1; Described nickel salt is Nickel dichloride hexahydrate, Nickelous nitrate hexahydrate, six hydration nickel sulfate; Mix slaine and be selected from hydrochloride, nitrate, sulfate; Mix metallic element and be selected from three kinds of combinations in cobalt, manganese, yttrium, lutetium, cadmium, the ytterbium; The particle diameter of this combination electrode material is 30～50nm.
Embodiment 3:As different from Example 1, the configuration nickel salt and mix in the mixed aqueous solution of slaine, total mol ratio of mixing metallic element and nickel element is 1:9; Described nickel salt is Nickel dichloride hexahydrate; Mix slaine and be selected from hydrochloride; Mixing metallic element is cobalt, manganese, yttrium, lutetium, cadmium, ytterbium; The particle diameter of this combination electrode material is 30～50nm.
Embodiment 4:As different from Example 1, the configuration nickel salt and mix in the mixed aqueous solution of slaine, total mol ratio of mixing metallic element and nickel element is 1:5; Described nickel salt is six hydration nickel sulfate; Mix slaine and be selected from hydrochloride; Mix metallic element and be in cobalt and manganese and yttrium and the cadmium one or more.
Be described further as follows to this bright a kind of nano nickel oxide composite electrode compounding method for ultracapacitor in conjunction with the embodiments:
Embodiment 5:Be used for the nano nickel oxide composite electrode compounding method of ultracapacitor, its processing step is as follows:
1) configuration nickel salt and the aqueous solution that mixes slaine, the slaine total concentration is 0.01～1mol/L, total mol ratio of wherein mixing metallic element and nickel element is 1:1～9; The described metallic element that mixes is one or more combinations in cobalt, manganese, yttrium, lutetium, cadmium, the ytterbium; The total mol ratio of present embodiment is 1:9; The described metallic element that mixes is selected from cobalt, also can be a kind of in manganese, yttrium, lutetium, cadmium, the ytterbium;
2) adding volume in the above-mentioned aqueous solution is the organic solvent of 0.1～4 times of aqueous solvent volume, obtains mixed solution A; It is the organic solvent of 3 times of aqueous solvent volumes that present embodiment adds volume in the above-mentioned aqueous solution.Described organic solvent is one or more the mixing in alcohols and the organic solvent of ketone.The present embodiment organic solvent is a kind of in methyl alcohol, ethanol, isopropyl alcohol or the acetone, also can be several mixing.
3) aqueous solution of configuration carbonic hydroammonium, then adding volume is the organic solvent of 0.1～4 times of aqueous solvent volume, obtains mixed solution B, and wherein the concentration of carbonic hydroammonium is 0.01～1mol/L, and the kind of organic solvent is consistent with mixed solution A; The aqueous solution of present embodiment configuration carbonic hydroammonium, then adding volume is the organic solvent of 2 times of aqueous solvent volumes;
4) above-mentioned mixed solution A was stirred 10～60 minutes, present embodiment is 30 minutes; Add fast subsequently mixed solution B and stirring within 30～300 seconds time, the pH value of control solution is 7～9, and the reaction time was at 1～3 hour;
5) above-mentioned reaction is carried out Separation of Solid and Liquid to slurry after finishing, and precipitation is washed with water 2～5 times, and in 50～150 ℃ of dryings 5～24 hours, present embodiment obtained calcining precursor in 100 ℃ of dryings 12 hours;
6) above-mentioned calcining precursor was calcined 2～6 hours under 250～450 ℃, namely make particle diameter at the nano nickel oxide composite electrode material of 30～50nm, present embodiment is calcined above-mentioned calcining precursor 23 hours under 3500 ℃, namely make particle diameter at the nano nickel oxide composite electrode material of 30～45nm, make electrode take prepared material as active material with conventional method again.
The making of nickel oxide combination electrode and performance test:
The nano nickel oxide composite electrode material that makes in the embodiment 1,2 or 3 respectively is as active material, conductive carbon black is conductive agent, PTFE (polytetrafluoroethylene) is binding agent, active material, conductive agent and binding agent mix in the ratio of 75:20:5, add to be coated on the nickel foam substrate equably after water stirs into paste.After 2～5 hours, with the pole piece hydrostatic profile, the lug of burn-oning namely makes nickel oxide electrode under the pressure of 12～18Mpa 65 ℃ of lower dryings.Adopt three-electrode system to carry out charge-discharge test, work electrode is above-mentioned nickel oxide combination electrode, is platinum electrode to electrode, and reference electrode is the Hg/HgO electrode, and electrolyte is the KOH solution of 6mol/L.Can calculate the specific capacity of nano nickel oxide composite electrode material under the different discharge current densities according to the result of charge-discharge test, the weight of nano nickel oxide composite electrode material, concrete outcome sees Table 1.
The specific capacity (F/g) of nano nickel oxide composite electrode material under the different discharge current densities of table 1
Claim protection range of the present invention is not limited to above-described embodiment.
Claims (6)
1. nano nickel oxide composite electrode that is used for ultracapacitor is characterized in that: it is to mix a certain amount of metallic element and the composite material made in Powdered nano oxidized nickel material that its system is joined material; Describedly in Powdered nano oxidized nickel material, mix a certain amount of metallic element, its metallic element incorporation is: the configuration nickel salt and mix in the mixed aqueous solution of slaine, the slaine total concentration is 0.01～1mol/L, and total mol ratio of wherein mixing metallic element and nickel element is 1:2; Described nickel salt is two kinds of Nickel dichloride hexahydrate, Nickelous nitrate hexahydrates; The described slaine that mixes is two kinds in hydrochloride, nitrate; The described metallic element that mixes is selected from cobalt, manganese, yttrium, lutetium, cadmium, the ytterbium two kinds; The particle diameter of combination electrode material is 40～50nm.
2. nano nickel oxide composite electrode that is used for ultracapacitor is characterized in that: it is to mix a certain amount of metallic element and the composite material made in Powdered nano oxidized nickel material that its system is joined material; Describedly in Powdered nano oxidized nickel material, mix a certain amount of metallic element, its metallic element incorporation is: the configuration nickel salt and mix in the mixed aqueous solution of slaine, the slaine total concentration is 0.01～1mol/L, and total mol ratio of mixing metallic element and nickel element is 1:9; Described nickel salt is Nickel dichloride hexahydrate; Mix slaine and be selected from hydrochloride; Mixing metallic element is cobalt, manganese, yttrium, lutetium, cadmium, ytterbium; The particle diameter of this combination electrode material is 30～50nm.
3. nano nickel oxide composite electrode that is used for ultracapacitor is characterized in that: it is to mix a certain amount of metallic element and the composite material made in Powdered nano oxidized nickel material that its system is joined material; Describedly in Powdered nano oxidized nickel material, mix a certain amount of metallic element, its metallic element incorporation is: the configuration nickel salt and mix in the mixed aqueous solution of slaine, the slaine total concentration is 0.01～1mol/L, and total mol ratio of mixing metallic element and nickel element is 1:5; Described nickel salt is six hydration nickel sulfate; Mix slaine and be selected from hydrochloride; Mixing metallic element is cobalt and manganese and yttrium and cadmium; The particle diameter of combination electrode material is 40～50nm.
4. a preparation method who is used for the nano nickel oxide composite electrode of ultracapacitor is characterized in that, it is to mix a certain amount of metallic element and the composite material made in Powdered nano oxidized nickel material that nano nickel oxide composite electrode system is joined material; Described metallic element is one or more combinations in cobalt, manganese, yttrium, lutetium, cadmium, the ytterbium; The preparation method comprises following processing step:
1) configuration nickel salt and the aqueous solution that mixes slaine, the slaine total concentration is 0.01～1mol/L, total mol ratio of wherein mixing metallic element and nickel element is 1:1～9; The described metallic element that mixes is one or more combinations in cobalt, manganese, yttrium, lutetium, cadmium, the ytterbium;
2) adding volume in the above-mentioned aqueous solution is the organic solvent of 0.1～4 times of aqueous solvent volume, obtains mixed solution A;
3) aqueous solution of configuration carbonic hydroammonium, then adding volume is the organic solvent of 0.1～4 times of aqueous solvent volume, obtains mixed solution B, wherein the concentration of carbonic hydroammonium is 0.01～1mol/L, organic solvent
Kind is consistent with mixed solution A;
4) above-mentioned mixed solution A was stirred 10～60 minutes, add fast subsequently mixed solution B and stirring within 30～300 seconds time, the pH value of control solution is 7～9, and the reaction time was at 1～3 hour;
5) above-mentioned reaction is carried out Separation of Solid and Liquid to slurry after finishing, and precipitation is washed with water 2～5 times, in 50～150 ℃ of dryings 5～24 hours, obtains calcining presoma;
6) above-mentioned calcining presoma was calcined 2～6 hours under 250～450 ℃, namely made particle diameter at the nano nickel oxide composite electrode material of 30～50nm, make electrode take prepared material as active material with conventional method again.
5. the preparation method of the nano nickel oxide composite electrode for ultracapacitor as claimed in claim 4 is characterized in that, described organic solvent is one or more the mixing in alcohols and the organic solvent of ketone.
6. such as the preparation method of claim 4 or 5 described nano nickel oxide composite electrodes for ultracapacitor, it is characterized in that preparation process is:
1) configuration nickel salt and the aqueous solution that mixes slaine, the slaine total concentration is 0.01～1mol/L, total mol ratio of wherein mixing metallic element and nickel element is 1:9; The described metallic element that mixes is selected from cobalt, also can be a kind of in manganese, yttrium, lutetium, cadmium, the ytterbium;
2) adding volume in the above-mentioned aqueous solution is the absolute ethyl alcohol of 0.1～4 times of aqueous solvent volume, obtains disposing the alcohol of slaine-water mixed solution A;
3) aqueous solution of configuration carbonic hydroammonium, then adding volume is the absolute ethyl alcohol of 0.1～4 times of aqueous solvent volume, obtains mixed solution B, wherein the concentration of carbonic hydroammonium is 0.01～1mol/L;
4) above-mentioned mixed solution A was stirred 30 minutes, within 30～300 seconds time, add fast subsequently above-mentioned ammonium bicarbonate soln, i.e. mixed solution B and stirring, the pH value of control solution is 7～9, and the reaction time was at 1～3 hour;
5) above-mentioned reaction is carried out Separation of Solid and Liquid to slurry after finishing, and precipitation is washed with water 2～5 times, in 100 ℃ of dryings 12 hours, obtains calcining presoma;
6) above-mentioned calcining presoma was calcined 3 hours under 350 ℃, namely made particle diameter at the nano nickel oxide composite electrode material of 30～45nm, make electrode take prepared material as active material with conventional method again.
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| CN103663572A (en) * | 2012-09-11 | 2014-03-26 | 中国科学院上海硅酸盐研究所 | Preparation method of nickel oxide material with superhigh specific capacity |
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| CN101333008A (en) * | 2007-06-29 | 2008-12-31 | 江苏双登集团有限公司 | Method for preparing nanometer nickel oxide composite powder |
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