CN105895383B - A kind of supercapacitor alloy/amorphous nickel cobalt hydroxide combination electrode and preparation method thereof - Google Patents
A kind of supercapacitor alloy/amorphous nickel cobalt hydroxide combination electrode and preparation method thereof Download PDFInfo
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- CN105895383B CN105895383B CN201610220370.5A CN201610220370A CN105895383B CN 105895383 B CN105895383 B CN 105895383B CN 201610220370 A CN201610220370 A CN 201610220370A CN 105895383 B CN105895383 B CN 105895383B
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- 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 discloses a kind of supercapacitor alloy/amorphous nickel cobalt hydroxide combination electrode preparation method, step includes: (1) cleaning foam metal；(2) foam metal based alloy is prepared；(3) the Electrodeposited Ni-Co hydroxide on foamed alloy；(4) metal/amorphous nickel cobalt hydroxide combination electrode is made.Meanwhile the invention also discloses combination electrodes obtained by above-mentioned preparation method.Compared with prior art, which can effectively improve the specific discharge capacity and cyclical stability of supercapacitor, have very high practical value and wide application prospect.
Description
Technical field
The present invention relates to a kind of combination electrodes, specifically, being to be related to a kind of supercapacitor alloy/amorphous nickel cobalt
Hydroxide combination electrode and preparation method thereof.
Background technique
Supercapacitor not only has the advantages that power density is high, energy density is big, charge-discharge velocity is fast, but also has
It is high-efficient, have extended cycle life, the advantages such as electrode material is environmentally protective and operating temperature range is wide, in information technology, mobile logical
, there is huge market potential in the fields such as news, electric car, fuel combination automobile, aerospace and science and techniques of defence, are current
The scientific research hot spot of society.
According to the difference of charge energy storage mechnism, supercapacitor can be divided into double layer capacitor and fake capacitance capacitor.?
In the electrode material of double layer capacitor, graphite is to study more and obtained the electrode material of business application, theoretical ratio
Capacity can achieve 400F/g.However, being influenced by pore-size distribution, configuration of surface and with factors such as electrolyte wellabilities, electricity
Lotus is obstructed in transmittance process, and a large amount of compound phenomenon occurs, and causing its actual specific capacity is only 200F/g or so.Transition
Metallic compound relies on its excellent fake capacitance characteristic, and good development trend, especially Ni have been showed in scientific research
(OH) 2 film of 2/Co (OH) has shown high initial mass specific capacity.However, fake capacitance electrode material is in charge and discharge
Cheng Zhong is limited by electrolyte ion orientation and charge migration rate, and the multiplying power property of high current charge-discharge is poor, limit
Further increasing for its chemical property is made.The fake capacitance characteristic for how giving full play to nickel cobalt metal is further to improve
The key of its chemical property and the emphasis of people's research.
Summary of the invention
The purpose of the present invention is to provide a kind of supercapacitor alloy/amorphous nickel cobalt hydroxide combination electrode, benefits
It has been obviously improved the electric conductivity of nickel cobalt hydroxide with foam metal based alloy, and then has promoted the quality specific volume of supercapacitor
Amount and cyclical stability.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of supercapacitor alloy/amorphous nickel cobalt hydroxide combination electrode, by foam metal based alloy and amorphous
Nickel cobalt hydroxide two parts are uniformly combined.
Further, the molecular formula of the amorphous nickel cobalt hydroxide is NixCoy(OH)2And x:y=1:(0.5 (x+y),
~2)。
The present invention additionally provides above-mentioned supercapacitor alloy/amorphous nickel cobalt hydroxide combination electrode system simultaneously
Preparation Method includes the following steps:
(1) foam metal is put into concentrated hydrochloric acid and is cleaned by ultrasonic, remove the oxide skin(coating) on foam metal surface, so
It is rinsed well afterwards with deionized water and ethyl alcohol；
(2) it uses metal salt solution or graphene suspension or carbon nano tube suspension as presoma, adjusts pH value of solution
Value, in situ electro-deposition prepares alloy/graphite alkene/carbon nano-tube film conductive layer on foam metal, then with deionized water and
Ethyl alcohol is rinsed well；
(3) step (2) resulting sample is placed in the in the mixed solvent of nickel salt and cobalt salt, adjusts pH value, it is in situ on it
Electric deposition nickel cobalt hydroxide；
(4) step (3) resulting sample is cleaned up with deionized water and ethyl alcohol, to get alloy/amorphous after drying
Nickel cobalt hydroxide combination electrode.
Further, in step (1), the foam metal is one of nickel foam, foam copper, foamed aluminium.It is described
The time of ultrasonic cleaning is 30min.
Further, in step (2), metal salt is silver nitrate, zinc nitrate, zinc sulfate, nitric acid in the presoma
Aluminium, aluminum sulfate, aluminium chloride, cobaltous iodide, cobaltous bromide, cobalt chloride, cobaltous fluoride, cobaltous sulfate, cobalt carbonate, cobalt nitrate, cobalt acetate, phosphorus
Sour cobalt, cobalt naphthenate, cobaltous octadecanate, new cobalt decanoate, cobalt boracylate, nickel iodide, nickelous bromide, nickel chloride, nickel fluoride, nickel sulfate,
One of ammonium nickel sulfate, nickelous carbonate, nickel nitrate, nickel acetate, citric acid nickel, nickel sulfide, copper chloride, copper nitrate, copper sulphate or
It is a variety of；The solvent of the presoma is water, methanol, ethyl alcohol, isopropanol, the tert-butyl alcohol, chloroform, ethylene glycol, dimethylacetamide
One of amine, dimethyl sulfoxide, benzyl ether, N-Methyl pyrrolidone, N- ethyl pyrrolidone, N,N-dimethylformamide are more
Kind；The concentration of the metal salt solution is 0.005 ~ 0.5mol/L, and the electrodeposition time is 1-100min.
Further, in step (2), the pH value of solution is adjusted to faintly acid, the pH adjusting agent with pH adjusting agent
For one or more of acetic acid, sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid.
Further, in step (3), the nickel salt is nickel iodide, nickelous bromide, nickel chloride, nickel fluoride, nickel sulfate, sulphur
One of sour nickel ammonium, nickelous carbonate, nickel nitrate, nickel acetate, citric acid nickel are a variety of；The cobalt salt is cobaltous iodide, cobaltous bromide, chlorine
Change cobalt, cobaltous fluoride, cobaltous sulfate, cobalt carbonate, cobalt nitrate, cobalt acetate, cobalt phosphate, cobalt naphthenate, cobaltous octadecanate, new cobalt decanoate, boron
One of acylated cobalt is a variety of；In the mixed solution of the nickel salt and cobalt salt, the chemical element metering ratio of nickel and cobalt is 1:2,
Its solvent is water, methanol, ethyl alcohol, isopropanol, the tert-butyl alcohol, chloroform, ethylene glycol, dimethyl acetamide, dimethyl sulfoxide, dibenzyl
One of ether, N-Methyl pyrrolidone, N- ethyl pyrrolidone, N,N-dimethylformamide are a variety of.
Still further, in step (3), using the pH value of electrolyte adjusting solution to 6 ~ 10, the electrolyte is carbon
One or more of sour sodium, sodium bicarbonate, sodium acetate, sodium phosphate, potassium carbonate etc.；The final solution of the step (3) is dense
Degree is 0.005 ~ 0.5mol/L, and the electrodeposition time is 1-100min
Preferably, in step (4), drying process carries out in vacuum environment or nitrogen protection environment, drying time
For 1~15h, drying temperature is 30~120 DEG C.
In the present invention, alloy/amorphous nickel cobalt hydroxide combination electrode high specific capacitance principle is: the height of nickel cobalt is counterfeit
The high conductivity of capacitor reserves and alloy.Wherein, the nickle atom and cobalt atom of transition group each provide enough oxidations
Reduction activation point, ensure that fake capacitance capacity；The high conductivity of foaming structure alloy, ensure that the fast exchange of its charge；It is special
It is not in alloy comprising being circulated throughout in capacitor charging/discharging different from nickel, the high activity of cobalt and when the third metal of high conductivity
Cheng Zhong, the third metal can participate in fake capacitance thermal energy storage process, be deposited on nickel cobalt hydroxide surfaces after uniform, to rise
The effect for exchanging and transmitting to rapid electric charge.
Compared with prior art, the invention has the following advantages:
(1) present invention is using the high fake capacitance reserves of nickel cobalt and the structure and high conductivity of alloy, with foam gold
Belong to and be used as skeleton, the foamed alloy of high-specific surface area and high conductivity is prepared by electrodeposition process in situ, then on foamed alloy
Electro-deposition amorphous nickel cobalt hydroxide in situ, finally through over cleaning, be dried to obtain combination electrode, preparation method science is closed
Reason, substantially increases the specific discharge capacity and cyclical stability of supercapacitor, has very high practical value and wide answers
Use prospect.
(2) in the present invention, the nickle atom and cobalt atom of transition group each provide enough redox actives
Point can fully ensure that the fake capacitance capacity of nickel cobalt metal, and then guarantee the smooth promotion of the chemical property of supercapacitor
With effectively improving for practical value.
(3) in the present invention, the high conductivity of foaming structure alloy ensure that the fast exchange of its charge；Especially foam
When constructional alloy includes the third metal different from nickel, the high activity of cobalt and high conductivity, followed in supercapacitor charge and discharge
During ring, which can participate in fake capacitance thermal energy storage process, equably be deposited on nickel cobalt hydroxide surfaces afterwards,
To play the effect for improving charge-exchange and transmission rate, so that the performance of supercapacitor has obtained significantly being promoted.
(4) preparation method of the present invention, reaction temperature is low, reaction is controllable, production safety hidden danger is not present, to life
The technical requirements of production personnel are not high, are very suitable to large-scale promotion application.
Specific embodiment
Below with reference to embodiment, the invention will be further described, and embodiments of the present invention are including but not limited to following
Embodiment.
Embodiment
Combination electrode disclosed by the invention, it is uniformly multiple by foam metal based alloy and amorphous nickel cobalt hydroxide two parts
It closes, wherein the molecular formula of amorphous nickel cobalt hydroxide is NixCoy(OH)2(x+y), and x:y=1:(0.5 ~ 2).This is multiple
Composite electrode compared with prior art, can not only effectively improve the specific discharge capacity and cyclical stability of supercapacitor, and
Preparation method is simple, is suitble to large-scale production and application.Preparation method can be summarized as following steps in general:
(1) foam metal is cleaned；
(2) foam metal based alloy is prepared；
(3) the Electrodeposited Ni-Co hydroxide on foamed alloy；
(4) metal/amorphous nickel cobalt hydroxide combination electrode is made.
In above-mentioned several steps, various aspects factor involved in each step there are many selection, especially selection,
In terms of the factors such as solution concentration and temperature, time, have extremely flexible variation space can basis in actual production
The needs of final products carry out free variation.Under above-mentioned principle, example is set forth below to illustrate the creativeness and reality of present aspect
With value.
Embodiment 1
Firstly, the nickel foam of 2cm*2cm*1.6mm is placed in ultrasonic cleaning 30min in 6Mol concentrated hydrochloric acid, de-soak is removed
The NiO layer of foam nickel surface, then rinsed well with deionized water and ethyl alcohol.Secondly, the sulfuric acid for being 0.01mol/L with 50ml concentration
For copper liquor as presoma, adjusting its pH value using sulfuric acid is 5.Then, using three-electrode method, the electricity in situ in nickel foam
Deposit the copper conductive layer of 20nm thickness；Wherein, the nickel foam cleaned up is made as working electrode, the Pt piece of 2cm*2cm*0.2mm
For to electrode, saturated calomel electrode is as reference electrode.The DC voltage of conducting -1V, at 25 DEG C, electro-deposition 5min；Again will
Obtained sample is cleaned up with deionized water and ethyl alcohol, and being placed in 20ml concentration is that 0.02mol/L nickel nitrate and 40ml are dense
Degree is to utilize sodium carbonate buffer, adjusting pH value to 9 or so, electro-deposition in the mixed aqueous solution of 0.04mol/L cobalt nitrate
5min, on it the nickel cobalt hydroxide of one layer of amorphous of electro-deposition in situ.Finally, by obtained sample deionized water and second
Alcohol cleans up, and dry 10h is under 60 DEG C of vacuum environments to get the Ni-based copper alloy of foam/nickel cobalt hydroxide combination electrode.
Manufactured combination electrode is assembled into three-electrode system and carries out performance detection, tests the electrode of super capacitor
Specific discharge capacity and charge-discharge performance.Test result: the Ni-based copper alloy of foam/amorphous nickel cobalt hydrogen manufactured in the present embodiment
Oxide combination electrode maximum specific capacity reaches 1258F/g；After circulation 2000 times, specific capacity keeps 95.3% or more.
Change the synthesis presoma ingredient and preparation condition of the Ni-based copper alloy of foam, other conditions are constant, obtained conjunction
Gold/amorphous nickel cobalt hydroxide combination electrode performance is as shown in table 1.As it can be seen from table 1 changing foam metal type, alloy
The factors such as presoma ingredient and pH value, electrodeposition time can significantly affect the specific discharge capacity and circulation of prepared combination electrode
Stability.Supporting substrate of the metal electrode as combination electrode among these, formation of the Structure and stability for combination electrode
Play a significant role with pattern；Conductive layer presoma ingredient and pH value directly determine the ingredient and uniformity of alloy nano-wire,
And then determine its facilitation to cobalt nickel fake capacitance performance；And electrodeposition time directly affects conductive layer thickness.Especially
, copper is since there are univalent copper ion and bivalent cupric ion, electro-chemical activity is higher.When containing copper in alloy, can participate in
Into the chemical reaction of nickel cobalt energy storage, it is obviously improved its charge-exchange and transmission rate, makes the electrochemical energy storage performance of nickel cobalt
It is not fully exerted, the specific discharge capacity because obtained from is higher.
Measurement result under 1 different-alloy of table and presoma ingredient, preparation condition
Embodiment 2
According to step described in embodiment 1, the copper of one layer of 20nm thickness of foam nickel surface electro-deposition after cleaning up is led
Electric layer.Then, obtained sample is placed in 20ml concentration is 0.02mol/L nickel nitrate and 40ml concentration is 0.04mol/L nitre
In the mixed aqueous solution of sour cobalt, using sodium carbonate buffer, pH value is adjusted to 9 or so, electro-deposition 5min, original position is electric on it
Deposit the nickel cobalt hydroxide of one layer of amorphous.Finally, obtained sample is cleaned up with deionized water and ethyl alcohol, 60
Dry 10h is under DEG C vacuum environment to get the Ni-based copper alloy of foam/nickel cobalt hydroxide combination electrode.Change nickel cobalt hydrogen-oxygen respectively
Ingredient, preparation condition and the drying condition of compound presoma keep other conditions constant, obtained electrode of super capacitor
Performance is as shown in table 2 below.
Measurement result under the different nickel cobalt hydroxide precursor ingredients of table 2, preparation condition and dry post-treatment condition
From table 2 it can be seen that changing the ingredient of presoma, preparation condition and dry post-treatment condition, can significantly affect
The specific discharge capacity and cyclical stability of obtained combination electrode, but change anyway, combination electrode produced by the present invention,
Its specific discharge capacity compared with prior art, all has and significantly improves, and be able to maintain a metastable cyclicity.
It can be seen that having very high compared with prior art, the present invention having substantive distinguishing features outstanding and significant technological progress
Creativeness.
Above-described embodiment is merely a preferred embodiment of the present invention, and it is not intended to limit the protection scope of the present invention, as long as using
Design principle of the invention, and the non-creative variation worked and made is carried out on this basis, it should belong to of the invention
Within protection scope.
Claims (10)
1. a kind of supercapacitor alloy/amorphous nickel cobalt hydroxide combination electrode, which is characterized in that closed by foam metal base
Gold is uniformly combined with amorphous nickel cobalt hydroxide two parts, includes different from nickel, cobalt in the foam metal based alloy
The third metal of high activity and high conductivity.
2. a kind of supercapacitor according to claim 1 alloy/amorphous nickel cobalt hydroxide combination electrode, feature
It is, the molecular formula of the amorphous nickel cobalt hydroxide is NixCoy (OH)2(x+y), and x:y=1:(0.5 ~ 2).
3. a kind of supercapacitor alloy/amorphous nickel cobalt hydroxide combination electrode preparation method, which is characterized in that including
Following steps:
(1) foam metal is put into concentrated hydrochloric acid and is cleaned by ultrasonic, removed the oxide skin(coating) on foam metal surface, then spend
Ionized water and ethyl alcohol are rinsed well；
(2) it uses metal salt solution as presoma, adjusts solution ph, original position electro-deposition prepares Thin film conductive on foam metal
Layer, is then rinsed well with deionized water and ethyl alcohol, obtains foam metal based alloy；
(3) step (2) resulting sample is placed in the in the mixed solvent of nickel salt and cobalt salt, adjusts pH value, electricity in situ is heavy on it
Product nickel cobalt hydroxide；
(4) step (3) resulting sample is cleaned up with deionized water and ethyl alcohol, to get alloy/amorphous nickel cobalt hydrogen after drying
Oxide combination electrode；
Wherein, the third metal different from nickel, the high activity of cobalt and high conductivity is included in the foam metal based alloy.
4. a kind of supercapacitor according to claim 3 alloy/amorphous nickel cobalt hydroxide combination electrode preparation
Method, which is characterized in that in step (1), the foam metal is one of nickel foam, foam copper, foamed aluminium.
5. a kind of supercapacitor according to claim 3 alloy/amorphous nickel cobalt hydroxide combination electrode preparation
Method, which is characterized in that in step (1), the time of the ultrasonic cleaning is 30min.
6. a kind of supercapacitor according to claim 3 alloy/amorphous nickel cobalt hydroxide combination electrode preparation
Method, which is characterized in that in step (2), in the presoma metal salt be silver nitrate, zinc nitrate, zinc sulfate, aluminum nitrate,
Aluminum sulfate, aluminium chloride, cobaltous iodide, cobaltous bromide, cobalt chloride, cobaltous fluoride, cobaltous sulfate, cobalt carbonate, cobalt nitrate, cobalt acetate, cobalt phosphate,
Cobalt naphthenate, cobaltous octadecanate, new cobalt decanoate, cobalt boracylate, nickel iodide, nickelous bromide, nickel chloride, nickel fluoride, nickel sulfate, nickel sulfate
One of ammonium, nickelous carbonate, nickel nitrate, nickel acetate, citric acid nickel, nickel sulfide, copper chloride, copper nitrate, copper sulphate are a variety of；Institute
The solvent for stating presoma is water, methanol, ethyl alcohol, isopropanol, the tert-butyl alcohol, chloroform, ethylene glycol, dimethyl acetamide, diformazan Asia
One of sulfone, benzyl ether, N-Methyl pyrrolidone, N- ethyl pyrrolidone, N,N-dimethylformamide are a variety of；The gold
The concentration for belonging to salting liquid is 0.005 ~ 0.5mol/L, and the electrodeposition time is 1-100min.
7. a kind of supercapacitor according to claim 3 alloy/amorphous nickel cobalt hydroxide combination electrode preparation
Method, which is characterized in that in step (2), the pH value of solution is adjusted to faintly acid with pH adjusting agent, the pH adjusting agent is
One or more of acetic acid, sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid.
8. a kind of supercapacitor according to claim 3 alloy/amorphous nickel cobalt hydroxide combination electrode preparation
Method, which is characterized in that in step (3), the nickel salt is nickel iodide, nickelous bromide, nickel chloride, nickel fluoride, nickel sulfate, sulfuric acid
One of nickel ammonium, nickelous carbonate, nickel nitrate, nickel acetate, citric acid nickel are a variety of；The cobalt salt is cobaltous iodide, cobaltous bromide, chlorination
Cobalt, cobaltous fluoride, cobaltous sulfate, cobalt carbonate, cobalt nitrate, cobalt acetate, cobalt phosphate, cobalt naphthenate, cobaltous octadecanate, new cobalt decanoate, boron acyl
Change one of cobalt or a variety of；In the mixed solution of the nickel salt and cobalt salt, the chemical element metering ratio of nickel and cobalt is 1:2,
Solvent be water, methanol, ethyl alcohol, isopropanol, the tert-butyl alcohol, chloroform, ethylene glycol, dimethyl acetamide, dimethyl sulfoxide, benzyl ether,
One of N-Methyl pyrrolidone, N- ethyl pyrrolidone, N,N-dimethylformamide are a variety of.
9. a kind of supercapacitor according to claim 3 alloy/amorphous nickel cobalt hydroxide combination electrode preparation
Method, which is characterized in that in step (3), using the pH value of electrolyte adjusting solution to 6 ~ 10, the electrolyte is carbonic acid
One or more of sodium, sodium bicarbonate, sodium acetate, sodium phosphate, potassium carbonate etc.；The final solution concentration of the step (3)
For 0.005 ~ 0.5mol/L, the electrodeposition time is 1-100min.
10. a kind of supercapacitor according to claim 3 alloy/amorphous nickel cobalt hydroxide combination electrode preparation
Method, which is characterized in that in step (4), drying process carries out in vacuum environment or nitrogen protection environment, drying time
For 1 ~ 15h, drying temperature is 30 ~ 120 DEG C.
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| CN106847530A (en) * | 2017-02-27 | 2017-06-13 | 四川大学 | A kind of nickel cobalt base-carbon nano tube combination electrode material and preparation method thereof |
| CN107658151B (en) * | 2017-10-18 | 2019-05-14 | 德清鼎兴电子有限公司 | A kind of foam ambrose alloy super capacitor electrode and its preparation process |
| CN108878163B (en) * | 2018-06-08 | 2020-08-04 | 太原理工大学 | Shape-controllable zinc-cobalt double hydroxide electrode material used as supercapacitor and preparation method thereof |
| CN110047658B (en) * | 2019-03-15 | 2021-02-26 | 四川大学 | Carbon and sulfur double-doped electrode material and preparation method thereof |
| CN112820554B (en) * | 2020-06-22 | 2022-07-26 | 深圳大学 | Nickel-cobalt hydroxide composite material, preparation method thereof and supercapacitor |
| CN112271084A (en) * | 2020-10-15 | 2021-01-26 | 同济大学 | Preparation method of nickel-cobalt hydroxide composite electrode material with high area capacity and high load capacity |
| CN112551650B (en) * | 2020-10-16 | 2022-11-04 | 北京工业大学 | Preparation method and application of foamed nickel loaded carbon nanotube/copper electrode for water treatment |
| CN114016103B (en) * | 2021-10-28 | 2022-11-01 | 浙江大学 | Amorphous transition metal hydroxide electrode material and preparation method thereof |
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| CN103985560B (en) * | 2014-04-28 | 2016-07-06 | 北京化工大学 | Brucite/CNT/nickel multilevel hierarchy thin film and its preparation method and application |
| CN105070515A (en) * | 2015-08-19 | 2015-11-18 | 华东理工大学 | Foamed nickel composite material, and preparation method and application thereof |
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