CN103440998B - A kind of cobalt acid zinc nanometer sheet array/nickel foam combination electrode, preparation method and application thereof - Google Patents
A kind of cobalt acid zinc nanometer sheet array/nickel foam combination electrode, preparation method and application thereof Download PDFInfo
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- CN103440998B CN103440998B CN201310366652.2A CN201310366652A CN103440998B CN 103440998 B CN103440998 B CN 103440998B CN 201310366652 A CN201310366652 A CN 201310366652A CN 103440998 B CN103440998 B CN 103440998B
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- Y02E60/13—Energy storage using capacitors
Abstract
A kind of cobalt acid zinc nanometer sheet array/nickel foam combination electrode, preparation method and application thereof, belong to energy storage technical field. Specifically zinc nitrate, cobalt nitrate, ammonium fluoride and urea are dissolved in the mixed solution of deionized water and alcohol (alcohol is one or more in methyl alcohol, ethanol or isopropyl alcohol) composition, stir; Nickel foam is immersed in this solution, carries out hydro-thermal reaction, naturally cooling, washing obtains cobalt acid zinc nanometer sheet array/nickel foam combination electrode after being dried, calcining. The cobalt acid zinc nanometer sheet that the present invention obtains vertically or is obliquely grown in surface the firmly combination with it of nickel foam, and be interconnected with one another, form nanometer sheet array, this has not only increased the contact area of electrolyte and nanometer sheet, but also has increased the stability of nanometer sheet array and whole electrode. Combination electrode is tested as ultracapacitor working electrode, under high current density condition, still can be there is higher specific capacitance and cyclical stability.
Description
Technical field
The invention belongs to energy storage technical field, particularly a kind of cobalt acid zinc nanometer sheet array/nickel foam is compoundElectrode, preparation method and the application in 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 effective, clean and continuable energy, and corresponding energyStorage and transformation technology. As energy storage of new generation and reforming unit, ultracapacitor, claims again electrochemistry electricityContainer, because it is safe, can fast charging and discharging and the outstanding advantages such as have extended cycle life be more and more subject to sectionScholar's extensive concern.
But ultracapacitor is due to low great its application at energy field that limited of energy density. Thereby asThe energy density what improves ultracapacitor has just become present scientist's problem demanding prompt solution. Solve super capacitorThe low key of device energy density is to develop the electrode material with excellent electrochemical character. Traditional super capacitorThe preparation method of device electrode is: first a certain amount of active material, adhesive and conductive agent are mixed, soAfter to be coated onto collector (as nickel foam etc.) upper, be pressed on subsequently under certain pressure finalObtain electrode of super capacitor. This method manufacturing process is very loaded down with trivial details, wayward, and the adding of adhesiveEnter the internal resistance that has greatly increased active material, the more important thing is because needs are suppressed under certain pressure,Cause the utilization rate of active material to reduce.
Transition metal oxide is in recent years because it has compared with high ratio capacitance and be subject to people compared with conventional carbon materialPay close attention to widely, as cobaltosic oxide, manganese dioxide and nickel oxide etc. But these transition metal oxidesConventionally there is the shortcomings such as poorly conductive, cyclical stability be undesirable. And cobalt acid zinc is as a kind of lithium ion of excellenceBattery material has received people's concern in recent years, but its application in ultracapacitor field seldom causes peopleAttention.
In patent (CN102664103A), disclose one makes cobalt acid zinc nanorod growth in nickel foamBecome the method for cobalt acid zinc nanometer rods/nickel foam combination electrode. But the cobalt obtaining by the method acid zinc nanometer rods alsoBe not the surface that is grown in an orderly manner nickel foam, do not form nanometer rods array, and using this combination electrode asThe ratio capacitance obtaining when ultracapacitor working 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 andIts application in ultracapacitor field.
Cobalt acid zinc nanometer sheet array/nickel foam combination electrode of the present invention is to adopt hydro-thermal method directly by cobalt acidZinc nanometer sheet vertically or is obliquely grown on the surface of nickel foam, forms orderly nanometer sheet array, by forgingBurning obtains cobalt acid zinc nanometer sheet array/nickel foam combination electrode. Cobalt acid zinc nanometer sheet array that the method is obtained/Nickel foam combination electrode, as ultracapacitor working electrode, still can have higher under high current density conditionSpecific capacitance and cyclical stability.
For reaching above-mentioned purpose, the preparation side of cobalt acid zinc nanometer sheet array/nickel foam combination electrode of the present inventionMethod, comprises the following steps:
1) by 0.25~1mmol zinc nitrate, 0.5~2mmol cobalt nitrate, 1.3~5mmol ammonium fluoride and2.5~10mmol urea is dissolved in deionized water and alcohol, and (alcohol is in methyl alcohol, ethanol, isopropyl alcoholOne or more) composition mixed solution in, stir;
2) above-mentioned solution is poured in teflon-lined stainless steel cauldron, will be cleaned also dried simultaneouslyNickel foam be immersed in this solution, after reactor sealing, carry out hydro-thermal reaction, then naturally cooling,After washing is dry, obtain the long nickel foam that has nanometer sheet array;
3) above-mentioned length there is is the nickel foam of nanometer sheet array calcine, obtain cobalt acid zinc nanometer sheet array/nickel foam multipleComposite electrode.
Improve as one, the volume ratio of deionized water and alcohol is 4:1~2:3;
Improve as one, the temperature of hydro-thermal reaction is 100~160 DEG C, and the reaction time is 3.5~8 hours;
Improve as one, calcining heat is 350~500 DEG C, and calcination time is 2~4 hours.
Beneficial effect of the present invention is:
(1) prepare the defect of ultracapacitor working electrode for tradition, the present invention does not need to add any conductionAgent and adhesive, be grown in cobalt acid zinc nanometer sheet array the surface of nickel foam equably by simple hydro-thermal method,And it is directly used as the working electrode of ultracapacitor, avoid traditional electrode of super capacitor to prepareComplicated processes.
(2) because cobalt acid zinc nanometer sheet is vertically or to be obliquely grown in 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 net of formationShape structure, thus utilization rate and the electric conductivity of active material improved, be convenient to electric transmission, and increase greatlyThe strong stability of electrode material; In addition, because nanometer sheet is to be evenly distributed in an orderly manner nickel foam surface, because ofAnd nanometer sheet array can contact fully with electrolyte, this has increased cobalt acid zinc active material and electrolyte greatlyContact area, improved its utilization rate, thereby can obtain excellent chemical property.
(3) cobalt acid zinc nanometer sheet array/nickel foam combination electrode the present invention being obtained carries out electro-chemical test,Current density be respectively 5,8,15,20,40,60,80 and 100A/g under carry out constant current charge-discharge surveyExamination has obtained respectively 2468,2382,2217,2128,1904,1740,1616 and the ratio of 1482F/gCapacitance. Under the high current densities of 30A/g, carry out cyclical stability test 1500 times, still can keep96.3% specific capacitance. The chemical property of above-mentioned excellence shows that kind electrode material is in ultracapacitor fieldThere is huge potential using value.
(4) the present invention is simple, and raw material is cheap, only can obtain preparation technology by simple two-step methodSimply, flow process is short, device dependence is low, is suitable for developing large-scale industrialization production application.
Brief description of the drawings
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.
Detailed description of the invention
The invention will be further described for following examples, but content of the present invention is not subject to the limit of this embodimentSystem.
Embodiment 1:
Step 1: under room temperature by 0.5mmol zinc nitrate, 1mmol cobalt nitrate, 2.5mmol ammonium fluoride and5mmol urea is dissolved in the mixed solution of 60mL deionized water and 40mL ethanol composition, stirs;
Step 2: above-mentioned solution is poured in teflon-lined stainless steel cauldron, will be cleaned also simultaneouslyDried nickel foam immerses in this solution, and reactor is sealed, and this reactor is put into the baking oven of 120 DEG CReact 4 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nanometer sheet that hasThe nickel foam of array;
Step 3: there is the nickel foam of nanometer sheet array to put at 350 DEG C of Muffle furnaces above-mentioned length and calcine 2 hours,Obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
Can find out from ESEM Fig. 1, Fig. 2 and Fig. 3, what obtain is cobalt acid zinc nanometer sheet array, this nanometer sheetBe grown in more uniformly in nickel foam substrate, nanometer sheet is vertical or favour the surface of nickel foam and nanometerSheet is interconnected with one another and forms array. In addition, the nanometer sheet thickness obtaining is about 10~50nm, is of a size of0.5~2μm。
Embodiment 2:
Step 1: under room temperature by 0.5mmol zinc nitrate, 1mmol cobalt nitrate, 2.5mmol ammonium fluoride and5mmol urea is dissolved in the mixed solution of 40mL deionized water and 60mL methyl alcohol composition, stirs;
Step 2: above-mentioned solution is poured in teflon-lined stainless steel cauldron, will be cleaned also simultaneouslyDried nickel foam immerses in this solution, and reactor is sealed, and this reactor is put into the baking oven of 120 DEG CReact 4.5 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nanometer that hasThe nickel foam of sheet array;
Step 3: there is the nickel foam of nanometer sheet array to put at 350 DEG C of Muffle furnaces above-mentioned length and calcine 4 hours,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 by 0.5mmol zinc nitrate, 1mmol cobalt nitrate, 2.5mmol ammonium fluoride and5mmol urea is dissolved in the mixed solution of 50mL ionized water and 50mL isopropyl alcohol composition, stirs;
Step 2: above-mentioned solution is poured in teflon-lined stainless steel cauldron, will be cleaned also simultaneouslyDried nickel foam immerses in this solution, and reactor is sealed, and this reactor is put into the baking oven of 120 DEG CReact 4 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nanometer sheet that hasThe nickel foam of array;
Step 3: there is the nickel foam of nanometer sheet array to put at 500 DEG C of Muffle furnaces above-mentioned length and calcine 2 hours,Obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
It is basic identical that the nanometer sheet obtaining under embodiment 3 conditions and embodiment 1 obtain, but embodiment 3 obtainsNanometer sheet can overlap.
Embodiment 4:
Step 1: under room temperature by 0.5mmol zinc nitrate, 1mmol cobalt nitrate, 2.5mmol ammonium fluoride and5mmol urea is 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 teflon-lined stainless steel cauldron, will be cleaned also simultaneouslyDried nickel foam immerses in this solution, and reactor is sealed, and this reactor is put into the baking oven of 120 DEG CReact 4 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nanometer sheet that hasThe nickel foam of array;
Step 3: there is the nickel foam of nanometer sheet array to put at 400 DEG C of Muffle furnaces above-mentioned length and calcine 2 hours,Obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
Embodiment 4 also can obtain nanometer sheet array, and the nanometer sheet just obtaining is the nanometer sheet circumnutating, and sizeEmbodiment 1 is less relatively, thinner thickness. The presentation of results deionized water of embodiment 4 and the ratio of alcohol are to nanometer sheetPattern and size have impact.
Embodiment 5:
Step 1: under room temperature by 1mmol zinc nitrate, 2mmol cobalt nitrate, 5mmol ammonium fluoride and 10mmolIt is molten that urea is dissolved in the mixing of 50mL deionized water, 20mL methyl alcohol, 20mL ethanol and 10mL isopropyl alcohol compositionIn liquid, stir;
Step 2: above-mentioned solution is poured in teflon-lined stainless steel cauldron, will be cleaned also simultaneouslyDried nickel foam immerses in this solution, and reactor is sealed, and this reactor is put into the baking oven of 120 DEG CReact 3.5 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nanometer that hasThe nickel foam of sheet array;
Step 3: there is the nickel foam of nanometer sheet array to put at 450 DEG C of Muffle furnaces above-mentioned length and calcine 2 hours,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 by 0.25mmol zinc nitrate, 0.5mmol cobalt nitrate, 1.3mmol ammonium fluoride and2.5mmol urea is 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 teflon-lined stainless steel cauldron, will be cleaned also simultaneouslyDried nickel foam immerses in this solution, and reactor is sealed, and this reactor is put into the baking oven of 160 DEG CReact 6 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nanometer sheet that hasThe nickel foam of array;
Step 3: there is the nickel foam of nanometer sheet array to put at 450 DEG C of Muffle furnaces above-mentioned length and calcine 2.5 hours,Obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
The nanometer sheet array growth obtaining under embodiment 6 conditions is comparatively intensive, and size is little compared with embodiment 1, pointCloth is not very even.
Embodiment 7:
Step 1: under room temperature by 0.5mmol zinc nitrate, 1mmol cobalt nitrate, 2.5mmol ammonium fluoride and5mmol urea is dissolved in the mixed solution of 60mL deionized water, 30mL ethanol and 10mL isopropyl alcohol composition;
Step 2: above-mentioned solution is poured in teflon-lined stainless steel cauldron, will be cleaned also simultaneouslyDried nickel foam immerses in this solution, and reactor is sealed, and this reactor is put into the baking oven of 100 DEG CReact 8 hours, naturally cooling, take out water and ethanol washing several respectively, and dry, obtain the long nanometer sheet that hasThe nickel foam of array;
Step 3: there is the nickel foam of nanometer sheet array to put at 350 DEG C of Muffle furnaces above-mentioned length and calcine 2 hours,Obtain cobalt acid zinc nanometer sheet array/nickel foam combination electrode.
Under embodiment 7 conditions, still can obtain nanometer sheet similar to Example 1, the nanometer sheet just obtaining withIt is relatively little that embodiment 1 compares size, and nanometer sheet overlaps.
Electrochemical properties test:
Cobalt acid zinc nanometer sheet array/nickel foam combination electrode that embodiment 1 is obtained is directly as ultracapacitor workCarry out electro-chemical test as electrode.
By this electrode respectively current density be 5,8,15,20,40,60,80 and 100A/g under carry outConstant current charge-discharge test. 1500 circulations are carried out in cyclical stability test under 30A/g current density conditionTest. Constant current charge-discharge test and cyclical stability test all adopt three electrode test systems, with saturated calomelElectrode is reference electrode, and platinum plate electrode is to electrode, and cobalt acid zinc nanometer sheet array/nickel foam combination electrode is directly doneFor working electrode. Electrolyte is the potassium hydroxide of 2mol/L, and test is carried out on Shanghai occasion China work station.
The electrode that Fig. 4 obtains for embodiment 1 as the current density of ultracapacitor working electrode with than electric capacityMagnitude relation figure as can be seen from the figure, is 5,8,15,20,40,60,80 and 100 in current densityThe ratio capacitance arriving under A/g condition 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 obtainingStill up to 1482F/g, the material that so large specific capacitance obtains has excellent ultracapacitorEnergy. Fig. 5 is cyclical stability resolution chart, as can be seen from the figure, under the high current density of 30A/g, carries outCyclical stability test, after 1500 circulations, specific capacitance still can keep 96.3%, and the electricity obtaining is describedUtmost point material has stable cyclical stability, and is adapted at discharging and recharging under large current condition.
The above, be only several case study on implementation of the present invention, not the present invention done any pro formaRestriction, although the present invention discloses as above with better case study on implementation, but be not in order to limit the present invention, anyThose skilled in the art, do not departing within the scope of technical solution of the present invention, when utilizing above-mentioned announcementStructure and technology contents are made a little change or are modified to the equivalent case study on implementation of equivalent variations. But it is not everyDepart from the content of technical solution of the present invention, that according to technical spirit of the present invention, above case study on implementation is done is anySimple modification, equivalent variations and modification, all still belong within the scope of technical solution of the present invention.
Claims (7)
1. a preparation method for cobalt acid zinc nanometer sheet array/nickel foam combination electrode, its step is as follows:
1) by 0.25~1mmol zinc nitrate, 0.5~2mmol cobalt nitrate, 1.3~5mmol ammonium fluoride and2.5~10mmol urea is dissolved in the mixed solution of deionized water and alcohol composition, stirs;
2) be immersed in above-mentioned mixed solution cleaning also dried nickel foam, carry out hydro-thermal reaction, thenNaturally cooling, after washing is dry, obtain the long nickel foam that has nanometer sheet array;
3) above-mentioned length there is is the nickel foam of nanometer sheet array calcine, obtain cobalt acid zinc nanometer sheet array/nickel foam multipleComposite electrode.
2. the preparation method of a kind of cobalt acid zinc nanometer sheet array/nickel foam combination electrode as claimed in claim 1, itsBe characterised 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/nickel foam combination electrode as claimed in claim 1, itsBe characterised in that: the volume ratio of deionized water and alcohol is 4:1~2:3.
4. the preparation method of a kind of cobalt acid zinc nanometer sheet array/nickel foam combination electrode as claimed in claim 1, itsBe characterised in that: the temperature of hydro-thermal reaction is 100~160 DEG C, the reaction time is 3.5~8 hours.
5. the preparation method of a kind of cobalt acid zinc nanometer sheet array/nickel foam combination electrode as claimed in claim 1, itsBe characterised in that: the temperature of calcining is 350~500 DEG C, calcination time is 2~4 hours.
6. cobalt acid zinc nanometer sheet array/nickel foam combination electrode, is characterized in that: be by claim 1~5 timesMethod described in what one prepares.
7. cobalt claimed in claim 6 acid zinc nanometer sheet array/nickel foam combination electrode is in ultracapacitor fieldApplication.
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