CN103440998A - Zinc cobaltate nanosheet array/foamed nickel combined electrode, preparation method and application thereof - Google Patents
Zinc cobaltate nanosheet array/foamed nickel combined electrode, preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a zinc cobaltate nanosheet array/foamed nickel combined electrode, a preparation method and application of the zinc cobaltate nanosheet array/foamed nickel combined electrode, and belongs to the technical field of energy storage. The preparation method particularly comprises the steps of dissolving zinc nitrate, cobalt nitrate, ammonium fluoride and urea into a mixing solution composed of deionized water and alcohol (one or more kinds of methyl alcohol, ethyl alcohol or isopropyl alcohol), evenly mixing, then immersing foamed nickel into the solution, carrying out hydrothermal reaction, and obtaining the zinc cobaltate nanosheet array/foamed nickel combined electrode after natural cooling, washing drying and calcination. Zinc cobaltate nanosheets obtained through the preparation method perpendicularly or slantly grow on the surface of the foamed nickel and are firmly combined with the foamed nickel, the zinc cobaltate nanosheets and the foamed nickel are mutually connected to form a nanosheet array, therefore, the contact areas between an electrolyte and the nanosheets are increased, and the stability of the nanosheet array and the stability of the whole electrode are further improved. When the zinc cobaltate nanosheet array/foamed nickel combined electrode is tested as the work electrode of a supercapacitor, the high specific capacitance and the cycling stability can still be achieved under the large current density condition.
Description
Technical field
The invention belongs to the energy storage technical field, particularly a kind of cobalt acid zinc nanometer sheet array/nickel foam combination electrode, preparation method and the application in the ultracapacitor field thereof.
Background technology
Along with becoming increasingly conspicuous of the problem of exhaustion and environmental pollution etc. day by day of global warming, fossil fuel, people more and more exigence find a kind of effectively, the clean and continuable energy, and corresponding stored energy and transformation technology.As energy storage of new generation and reforming unit, ultracapacitor, claim again electrochemical capacitor, but more and more be subject to scientist's extensive concern because of its safe fast charging and discharging and the outstanding advantages such as have extended cycle life.
But ultracapacitor has limited its application at energy field greatly because energy density is low.Thereby the energy density that how to improve ultracapacitor has just become present scientist's problem demanding prompt solution.Solve the low key of super capacitor energy density and be to develop the electrode material with excellent electrochemical character.The preparation method of traditional electrode of super capacitor is: at first a certain amount of active material, adhesive and conductive agent are mixed, then it is coated onto to collector (as nickel foam etc.) upper, being pressed on subsequently under certain pressure finally obtains electrode of super capacitor.This method manufacturing process is very loaded down with trivial details, wayward, and adhesive add the internal resistance that has greatly increased active material, the more important thing is because needs are suppressed under certain pressure, cause the utilance of active material to reduce.
Transition metal oxide is subject to people and pays close attention to widely because it has higher ratio capacitance than the conventional carbon material in recent years, as cobaltosic oxide, manganese dioxide and nickel oxide etc.But there are the shortcomings such as poorly conductive, cyclical stability be undesirable usually in these transition metal oxides.And cobalt acid zinc has received people's concern in recent years as a kind of lithium ion battery material of excellence, but its application in the ultracapacitor field seldom attracts much attention.
A kind of method of cobalt acid zinc nanorod growth being made on nickel foam to cobalt acid zinc nanometer rods/nickel foam combination electrode is disclosed in patent (CN102664103A).But the cobalt obtained by the method acid zinc nanometer rods is not the surface that is grown in an orderly manner nickel foam, do not form the nanometer rods array, and the ratio capacitance obtained during using this combination electrode as the ultracapacitor work electrode is unsatisfactory, particularly under high current densities.
Summary of the invention
The object of the present invention is to provide a kind of cobalt acid zinc nanometer sheet array/nickel foam combination electrode, preparation method and the application in the ultracapacitor field thereof.
Cobalt acid zinc nanometer sheet array of the present invention/nickel foam combination electrode, to adopt hydro thermal method directly vertically or obliquely to be grown on the surface of nickel foam by cobalt acid zinc nanometer sheet, form orderly nanometer sheet array, by calcining, obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.The cobalt acid zinc nanometer sheet array that the method is obtained/nickel foam combination electrode, as the ultracapacitor work electrode, still can have higher specific capacitance and cyclical stability under the high current density condition.
For reaching above-mentioned purpose, the preparation method of cobalt acid zinc nanometer sheet array of the present invention/nickel foam combination electrode comprises the following steps:
1) 0.25～1mmol zinc nitrate, 0.5～2mmol cobalt nitrate, 1.3～5mmol ammonium fluoride and 2.5～10mmol urea are dissolved in the mixed solution of deionized water and alcohol (alcohol is one or more in methyl alcohol, ethanol, isopropyl alcohol) composition, stir;
2) above-mentioned solution is poured in the teflon-lined stainless steel cauldron, to clean also dried nickel foam is immersed in this solution simultaneously, carry out hydro-thermal reaction after the reactor sealing, then naturally cooling, obtain the long nickel foam that the nanometer sheet array is arranged after the washing drying;
3) above-mentioned length is had to the nickel foam calcining of nanometer sheet array, obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
As a kind of improvement, deionized water and pure volume ratio are 4:1～2:3;
As a kind of improvement, the temperature of hydro-thermal reaction is 100～160 ℃, and the reaction time is 3.5～8 hours;
As a kind of improvement, calcining heat is 350～500 ℃, and calcination time is 2～4 hours.
Beneficial effect of the present invention is:
(1) prepare the defect of ultracapacitor work electrode for tradition, the present invention does not need to add any conductive agent and adhesive, by simple hydro thermal method, cobalt acid zinc nanometer sheet array is grown in equably to the surface of nickel foam, and it is directly used to the complicated processes of having avoided traditional electrode of super capacitor to prepare as the work electrode of ultracapacitor.
(2) because cobalt acid zinc nanometer sheet is vertically or obliquely to be grown on nickel foam by gentle hydro thermal method, so nanometer sheet can be combined with nickel foam very securely, and nanometer sheet is interconnected with one another the orderly network structure of formation, thereby utilance and the conductivity of active material have been improved, be convenient to electric transmission, and strengthened greatly the stability of electrode material; In addition, because nanometer sheet is to be evenly distributed in an orderly manner the nickel foam surface, thereby the nanometer sheet array can contact fully with electrolyte, and this has increased the contact area of cobalt acid zinc active material and electrolyte greatly, improve its utilance, thereby can obtain excellent chemical property.
(3) cobalt that the present invention obtained acid zinc nanometer sheet array/nickel foam combination electrode carries out electro-chemical test, current density be respectively 5,8,15,20,40,60,80 and 100A/g under carry out the constant current charge-discharge test and obtained respectively 2468,2382,2217,2128,1904,1740,1616 and the specific capacitance of 1482F/g.Carry out cyclical stability test 1500 times under the high current densities of 30A/g, still can keep 96.3% specific capacitance.The chemical property of above-mentioned excellence shows that the kind electrode material has huge potential using value in the ultracapacitor field.
(4) the present invention is simple, and raw material is cheap, only by simple two-step method, can obtain, and preparation technology is simple, flow process is short, device dependence is low, is suitable for developing the large-scale industrialization production application.
The accompanying drawing explanation
Fig. 1: 430 times of scanning electron microscope diagrams that are coated with the nickel foam of cobalt acid zinc nanometer sheet;
Fig. 2: 5000 times of scanning electron microscope diagrams that are coated with the nickel foam of cobalt acid zinc nanometer sheet;
Fig. 3: 20000 times of scanning electron microscope diagrams that are coated with the nickel foam of cobalt acid zinc nanometer sheet;
Fig. 4: current density and the specific capacitance graph of a relation of cobalt acid zinc nanometer sheet array/nickel foam combination electrode;
Fig. 5: the stable circulation test result figure of cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
Embodiment
The invention will be further described for following examples, but content of the present invention is not subject to the restriction of this embodiment.
Embodiment 1:
Step 1: under room temperature, 0.5mmol zinc nitrate, 1mmol cobalt nitrate, 2.5mmol ammonium fluoride and 5mmol urea are dissolved in the mixed solution of 60mL deionized water and 40mL ethanol composition, stir;
Step 2: above-mentioned solution is poured in the teflon-lined stainless steel cauldron, to clean also dried nickel foam immerses in this solution simultaneously, and reactor is sealed, the baking oven that this reactor is put into to 120 ℃ reacts 4 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nickel foam that the nanometer sheet array is arranged;
Step 3: have the nickel foam of nanometer sheet array to put under 350 ℃ of Muffle furnaces calcining 2 hours above-mentioned length, obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
From ESEM Fig. 1, Fig. 2 and Fig. 3, can find out, what obtain is cobalt acid zinc nanometer sheet array, and this nanometer sheet is grown in the nickel foam substrate more uniformly, and nanometer sheet is vertical or favour the surface of nickel foam, and nanometer sheet is interconnected with one another and forms array.In addition, the nanometer sheet thickness obtained is about 10～50nm, is of a size of 0.5～2 μ m.
Embodiment 2:
Step 1: under room temperature, 0.5mmol zinc nitrate, 1mmol cobalt nitrate, 2.5mmol ammonium fluoride and 5mmol urea are dissolved in the mixed solution of 40mL deionized water and 60mL methyl alcohol composition, stir;
Step 2: above-mentioned solution is poured in the teflon-lined stainless steel cauldron, to clean also dried nickel foam immerses in this solution simultaneously, and reactor is sealed, the baking oven that this reactor is put into to 120 ℃ reacts 4.5 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nickel foam that the nanometer sheet array is arranged;
Step 3: have the nickel foam of nanometer sheet array to put under 350 ℃ of Muffle furnaces calcining 4 hours above-mentioned length, obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
The nanometer sheet array and the embodiment 1 that under embodiment 2 conditions, obtain are basically identical.
Embodiment 3:
Step 1: under room temperature, 0.5mmol zinc nitrate, 1mmol cobalt nitrate, 2.5mmol ammonium fluoride and 5mmol urea are dissolved in the mixed solution of 50mL ionized water and 50mL isopropyl alcohol composition, stir;
Step 2: above-mentioned solution is poured in the teflon-lined stainless steel cauldron, to clean also dried nickel foam immerses in this solution simultaneously, and reactor is sealed, the baking oven that this reactor is put into to 120 ℃ reacts 4 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nickel foam that the nanometer sheet array is arranged;
Step 3: have the nickel foam of nanometer sheet array to put under 500 ℃ of Muffle furnaces calcining 2 hours above-mentioned length, obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
The nanometer sheet and the embodiment 1 that under embodiment 3 conditions, obtain are resulting basic identical, but the nanometer sheet that embodiment 3 obtains can overlap.
Embodiment 4:
Step 1: under room temperature, 0.5mmol zinc nitrate, 1mmol cobalt nitrate, 2.5mmol ammonium fluoride and 5mmol urea are dissolved in the mixed solution of 80mL deionized water, 10mL methyl alcohol and 10mL ethanol composition, stir;
Step 2: above-mentioned solution is poured in the teflon-lined stainless steel cauldron, to clean also dried nickel foam immerses in this solution simultaneously, and reactor is sealed, the baking oven that this reactor is put into to 120 ℃ reacts 4 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nickel foam that the nanometer sheet array is arranged;
Step 3: have the nickel foam of nanometer sheet array to put under 400 ℃ of Muffle furnaces calcining 2 hours above-mentioned length, obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
Embodiment 4 also can obtain the nanometer sheet array, and the nanometer sheet just obtained is the nanometer sheet circumnutated, and the relative embodiment 1 of size is less, thinner thickness.The presentation of results deionized water of embodiment 4 and pure ratio are influential to pattern and the size of nanometer sheet.
Embodiment 5:
Step 1: under room temperature, 1mmol zinc nitrate, 2mmol cobalt nitrate, 5mmol ammonium fluoride and 10mmol urea are dissolved in the mixed solution of 50mL deionized water, 20mL methyl alcohol, 20mL ethanol and 10mL isopropyl alcohol composition, stir;
Step 2: above-mentioned solution is poured in the teflon-lined stainless steel cauldron, to clean also dried nickel foam immerses in this solution simultaneously, and reactor is sealed, the baking oven that this reactor is put into to 120 ℃ reacts 3.5 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nickel foam that the nanometer sheet array is arranged;
Step 3: have the nickel foam of nanometer sheet array to put under 450 ℃ of Muffle furnaces calcining 2 hours above-mentioned length, obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
Under embodiment 5 conditions also can to cobalt acid zinc nanometer sheet array.
Embodiment 6:
Step 1: under room temperature, 0.25mmol zinc nitrate, 0.5mmol cobalt nitrate, 1.3mmol ammonium fluoride and 2.5mmol urea are dissolved in the mixed solution of 60mL deionized water, 30mL ethanol and 10mL methyl alcohol composition, stir;
Step 2: above-mentioned solution is poured in the teflon-lined stainless steel cauldron, to clean also dried nickel foam immerses in this solution simultaneously, and reactor is sealed, the baking oven that this reactor is put into to 160 ℃ reacts 6 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nickel foam that the nanometer sheet array is arranged;
Step 3: have the nickel foam of nanometer sheet array to put under 450 ℃ of Muffle furnaces calcining 2.5 hours above-mentioned length, obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
The nanometer sheet array growth obtained under embodiment 6 conditions is comparatively intensive, and size is little than embodiment 1, and it is not very even distributing.
Embodiment 7:
Step 1: under room temperature, 0.5mmol zinc nitrate, 1mmol cobalt nitrate, 2.5mmol ammonium fluoride and 5mmol urea are dissolved in the mixed solution of 60mL deionized water, 30mL ethanol and 10mL isopropyl alcohol composition;
Step 2: above-mentioned solution is poured in the teflon-lined stainless steel cauldron, to clean also dried nickel foam immerses in this solution simultaneously, and reactor is sealed, the baking oven that this reactor is put into to 100 ℃ reacts 8 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nickel foam that the nanometer sheet array is arranged;
Step 3: have the nickel foam of nanometer sheet array to put under 350 ℃ of Muffle furnaces calcining 2 hours above-mentioned length, obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
Still can obtain nanometer sheet similar to Example 1 under embodiment 7 conditions, the nanometer sheet just obtained is compared the size less with embodiment 1, and nanometer sheet overlaps.
The electrochemical properties test:
The cobalt acid zinc nanometer sheet array that embodiment 1 is obtained/nickel foam combination electrode directly carries out electro-chemical test as the ultracapacitor work electrode.
By this electrode respectively current density be 5,8,15,20,40,60,80 and 100A/g under carry out the constant current charge-discharge test.1500 loop tests are carried out in the cyclical stability test under 30A/g current density condition.Constant current charge-discharge test and cyclical stability test all adopt three electrode test systems, take saturated calomel electrode as reference electrode, and platinum plate electrode is to electrode, and cobalt acid zinc nanometer sheet array/nickel foam combination electrode is directly as work electrode.The potassium hydroxide that electrolyte is 2mol/L, test is carried out on Shanghai occasion China work station.
Fig. 4 is current density and the specific capacitance graph of a relation of the resulting electrode of embodiment 1 as the ultracapacitor work electrode, as can be seen from the figure, current density be 5,8,15,20,40,60,80 and the 100A/g condition under the ratio capacitance arrived respectively up to 2468,2382,2217,2128,1904,1740,1616 and 1482F/g.Even under the super-large current density conditions of 100A/g, the specific capacitance obtained is still up to 1482F/g, and the material that so large specific capacitance obtains has excellent ultracapacitor performance.Fig. 5 is the cyclical stability resolution chart, as can be seen from the figure, carry out the cyclical stability test under the high current density of 30A/g, after 1500 circulations, specific capacitance still can keep 96.3%, illustrate that the electrode material obtained has stable cyclical stability, and be adapted at being discharged and recharged under large current condition.
The above, it is only several case study on implementation of the present invention, not the present invention is done to any pro forma restriction, although the present invention discloses as above with better case study on implementation, yet not in order to limit the present invention, any those skilled in the art, within not breaking away from the technical solution of the present invention scope, when the structure that can utilize above-mentioned announcement and technology contents are made a little change or be modified to the equivalent case study on implementation of equivalent variations.But every content that does not break away from technical solution of the present invention, any simple modification, equivalent variations and the modification above case study on implementation done according to technical spirit of the present invention, all still belong in the technical solution of the present invention scope.
Claims (7)
1. the preparation method of cobalt acid zinc nanometer sheet array/nickel foam combination electrode, its step is as follows:
1) 0.25～1mmol zinc nitrate, 0.5～2mmol cobalt nitrate, 1.3～5mmol ammonium fluoride and 2.5～10mmol urea are dissolved in the mixed solution of deionized water and alcohol composition, stir;
2) will clean also dried nickel foam and be immersed in above-mentioned mixed solution, carry out hydro-thermal reaction, then naturally cooling, obtain the long nickel foam that the nanometer sheet array is arranged after the washing drying;
3) above-mentioned length is had to the nickel foam calcining of nanometer sheet array, obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
2. the preparation method of a kind of cobalt acid zinc nanometer sheet array as claimed in claim 1/nickel foam combination electrode is characterized in that: alcohol is one or more in methyl alcohol, ethanol, isopropyl alcohol.
3. the preparation method of a kind of cobalt acid zinc nanometer sheet array as claimed in claim 1/nickel foam combination electrode is characterized in that: deionized water and pure volume ratio are 4:1～2:3.
4. the preparation method of a kind of cobalt acid zinc nanometer sheet array as claimed in claim 1/nickel foam combination electrode, it is characterized in that: the temperature of hydro-thermal reaction is 100～160 ℃, the reaction time is 3.5～8 hours.
5. the preparation method of a kind of cobalt acid zinc nanometer sheet array as claimed in claim 1/nickel foam combination electrode, it is characterized in that: the temperature of calcining is 350～500 ℃, calcination time is 2～4 hours.
6. cobalt acid zinc nanometer sheet array/nickel foam combination electrode, is characterized in that: be to be prepared by any one described method of claim 1～5.
7. the cobalt acid zinc nanometer sheet array claimed in claim 6/application of nickel foam combination electrode in the ultracapacitor field.
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| CN105244191A (en) * | 2015-10-27 | 2016-01-13 | 渤海大学 | Manganese cobalt oxide porous nanometer sheet/foam nickel compound electrode material preparation method |
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