CN102664103A - Zinc cobaltate nanorod/foam nickel composite electrode, preparation method thereof and application thereof - Google Patents
Zinc cobaltate nanorod/foam nickel composite electrode, preparation method thereof and application thereof Download PDFInfo
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- CN102664103A CN102664103A CN2012100926701A CN201210092670A CN102664103A CN 102664103 A CN102664103 A CN 102664103A CN 2012100926701 A CN2012100926701 A CN 2012100926701A CN 201210092670 A CN201210092670 A CN 201210092670A CN 102664103 A CN102664103 A CN 102664103A
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention provides a zinc cobaltate nanorod /foam nickel composite electrode, a preparation method thereof and application thereof. According to the method, a foam nickel plate is immersed in a mixed solution of zinc nitrate and cobalt nitrate, heating and heat preservation are carried out in order, an oxalic acid solution is added dropwise, reaction is carried out until the foam nickel grows a nanostructured precursor, the foam nickel is removed, and cleaning, drying and calcining are carried out in order to obtain the zinc cobaltate nanorod /foam nickel composite electrode. The composite electrode has properties of one-dimensional zinc cobaltate nano material with a large specific surface area and porous foam nickel, a contact area with an electrolyte is effectively increased, the electrode material is more fully involved in an electrochemical reaction, the composite electrode obtained through the reaction has a good electrochemical property and is applied in a super capacitor, the performance of a present capacitor is greatly raised, production process is simple, and the electrode is easy to be applied to the actual mass production.
Description
Technical field
The invention belongs to energy storage of new generation field, particularly a kind of cobalt acid zinc nanometer rods/nickel foam composite construction high power capacity ultracapacitor.
Background technology
Along with aspects such as communication, electronic equipment, auto industry and space technology develop rapidly, international energy problem in short supply has become increasingly conspicuous, and each state is all in the R and D that step up new forms of energy.In energy storage of new generation field; Ultracapacitor and lithium ion battery are indispensable parts; Be widely used in fields such as mobile phone, notebook computer and military equipment rapidly, bigger development space will be brought to ultracapacitor in the electric automobile field that enlarges day by day.Compare lithium ion battery, ultracapacitor has the huge advantage and the outstanding characteristic of the incomparable power aspect of other energy-storage travelling wave tubes.Though ultracapacitor has higher power density; But be not difficult under study for action to find that the capacitance of ultracapacitor under the high power situation and energy density are extremely low; Its reason is that this body structure of electrode is single; Conductivity, the contact of metal collector and material are relatively poor, owing to electrode destroyed cause that more greatly surface area is less than normal etc., this restricts it is greatly having bigger development on the electric automobile from now in the charge and discharge process.
Summary of the invention
The object of the present invention is to provide a kind of cobalt acid zinc nanometer rods/nickel foam combination electrode; Have the one dimension cobalt acid zinc nano material of bigger serface and the characteristic of loose porous nickel foam simultaneously; Can increase the contact area with electrolyte effectively, electrode material is participated in the middle of the electrochemical reaction more fully, make material have high electrochemical performance; And have good flexibility, adapt to following demand for the flexible foldable battery.
Another object of the present invention is to provide the method for the above-mentioned cobalt acid of preparation zinc nanometer rods/nickel foam combination electrode.
The 3rd purpose of the present invention is to provide the application of above-mentioned cobalt acid zinc nanometer rods/nickel foam combination electrode at ultracapacitor.
A kind of cobalt acid zinc nanometer rods/nickel foam combination electrode, growth has cobalt acid zinc nanometer rods on the nickel foam sheet.
A kind of method for preparing cobalt acid zinc nanometer rods/nickel foam combination electrode; Be specially: the nickel foam sheet is immersed in the mixed solution of zinc nitrate and cobalt nitrate; Insulation after being heated to 80 °-150 ℃ drips oxalic acid solution, and reaction grows the nanostructure presoma on nickel foam; The taking-up nickel foam is cleaned successively, is dried and calcining obtains cobalt acid zinc nanometer rods/nickel foam combination electrode.
Further, the mass concentration of said zinc nitrate and cobalt nitrate is respectively 0.008~0.034mol/L and 0.017~0.066mol/L;
Further, adopt the heating of back flow reaction stove;
Further, insulation is 1-2 hour;
Further, 300~500 ℃ of calcinings 2 hours of annealing down.
The cobalt acid zinc nanometer rods/application of nickel foam combination electrode in ultracapacitor is with its work electrode as ultracapacitor.
The present invention has following beneficial effect:
1. the present invention's nickel foam of adopting good conductivity and having a loose porous unique texture is as substrate; At surperficial direct growth cobalt acid zinc nano material; Help so practicing thrift very much employed conductive agent and binder material in the traditional electrode; The process of loaded down with trivial details making electrode slice has also been avoided in energy-conserving and environment-protective.Because active material is to produce on nickel foam, so that material contacts with substrate is very good, be convenient to strengthen electric transmission, help the cycle performance of ultracapacitor.The multistage composite structure of this novelty has very high practical value.
2. made composite construction has the one dimension cobalt acid zinc nano material of bigger serface and the characteristic of loose porous nickel foam simultaneously; Can increase contact area effectively with electrolyte; Electrode material is participated in the middle of the electrochemical reaction more fully, make material have high electrochemical performance.
3. the combination electrode that makes has good flexibility, can adapt to following demand for the flexible foldable battery;
4. cobalt acid zinc nanometer rods of the present invention/applied ultracapacitor of nickel foam combination electrode is carried out performance test, after 1000 charge and discharge cycles, capacitance still remains more than 97% of initial value, shows the cycle life that this ultracapacitor is good.High current density at 20A/g discharges and recharges down, and this ultracapacitor has up to the specific capacitance more than 1000, adapts to high-power application fully;
5. manufacturing process is simple, and raw material is cheap, only needs to adopt simple circumfluence method and the lower annealing process of temperature, and equipment requirements and cost are all lower, are suitable for large-scale promotion production.
Description of drawings
Fig. 1 is the scanning electron microscope diagram of pure foam nickel;
Fig. 2 is the long scanning electron microscope diagram that the nickel foam composite construction of cobalt acid zinc nanometer rods is arranged;
Fig. 3 has the scanning electron microscope diagram of the nickel foam composite construction of cobalt acid zinc nanometer rods for the length of amplifying;
Fig. 4 is ultracapacitor cycle performance test result figure.
Fig. 5 is ultracapacitor high rate performance test result figure.
Fig. 6 is ultracapacitor energy density and power density test result figure.
Embodiment
The present invention at first makes the long nickel foam that zinc cobalt oxygen presoma is arranged through circumfluence method, afterwards again through Muffle furnace annealing, with the abundant oxidation of presoma, makes the long nickel foam that zinc cobalt oxygen club shaped structure is arranged.
Below in conjunction with concrete embodiment technical scheme of the present invention is further described:
Embodiment 1:
1. at normal temperatures,, zinc nitrate and the cobalt nitrate concentration with 0.017mol/L and 0.033mol/L is dissolved in the deionized water simultaneously, processes solution A, and 3~4 nickel foam sheets (as shown in Figure 1) that sheared are immersed in this solution through abundant stirring;
2. at normal temperatures,, the concentration of oxalic acid with 0.3mol/L is dissolved in the deionized water, processes solution B through abundant stirring; (medicine of use is direct purchase, and the volume ratio of solution A, B is 3: 2)
3. solution A and nickel foam are added in the there-necked flask, with the heating of back flow reaction stove up to temperature stabilization at 80 ℃, the while stirs with Reasonable Speed;
4. be in the oxalic acid solution dropping entering flask of 0.2mol/L with concentration, and reacted 2 hours down at 80 ℃; The oxalic acid solution purpose is for making that reaction solution is acid, and zinc nitrate and cobalt nitrate be fully reaction under sour environment, grows the nanostructure presoma at the nickel foam sheet.
5. take out the nickel sheet, put into Muffle furnace after the clean dry and calcine.Annealed 120 minutes down at 300 ℃.Natural cooling promptly gets product (shown in Fig. 2 and 3) afterwards.
Embodiment 2:
1. at normal temperatures,, zinc nitrate and the cobalt nitrate concentration with 0.008mol/L and 0.017mol/L is dissolved in the deionized water simultaneously, processes solution A, and 3~4 nickel foam sheets that sheared are immersed in this solution through abundant stirring;
2. at normal temperatures,, the concentration of oxalic acid with 0.3mol/L is dissolved in the deionized water, processes solution B through abundant stirring; (medicine of use is direct purchase, and the volume ratio of solution A, B is 3: 2)
3. solution A and nickel foam are added in the there-necked flask, with the heating of back flow reaction stove up to temperature stabilization at 120 ℃, the while stirs with Reasonable Speed;
4. be in the oxalic acid solution dropping entering flask of 0.2mol/L with concentration, and reacted 2 hours down at 120 ℃; The oxalic acid solution purpose is for making that reaction solution is acid, and zinc nitrate and cobalt nitrate be fully reaction under sour environment, grows the nanostructure presoma at the nickel foam sheet.
5. take out the nickel sheet, put into Muffle furnace after the clean dry and calcine.Annealed 120 minutes down at 300 ℃.Natural cooling promptly gets product afterwards.
Embodiment 3:
1. at normal temperatures,, zinc nitrate and the cobalt nitrate concentration with 0.034mol/L and 0.066mol/L is dissolved in the deionized water simultaneously, processes solution A, and 3~4 nickel foam sheets that sheared are immersed in this solution through abundant stirring;
2. at normal temperatures,, the concentration of oxalic acid with 0.3mol/L is dissolved in the deionized water, processes solution B through abundant stirring; (medicine of use is direct purchase, and the volume ratio of solution A, B is 3: 2)
3. solution A and nickel foam are added in the there-necked flask, with the heating of back flow reaction stove up to temperature stabilization at 150 ℃, the while stirs with Reasonable Speed;
4. be in the oxalic acid solution dropping entering flask of 0.2mol/L with concentration, and reacted 2 hours down at 150 ℃; The oxalic acid solution purpose is for making that reaction solution is acid, and zinc nitrate and cobalt nitrate be fully reaction under sour environment, grows the nanostructure presoma at the nickel foam sheet.
5. take out the nickel sheet, put into Muffle furnace after the clean dry and calcine.Annealed 120 minutes down at 300 ℃.Natural cooling promptly gets product afterwards.
Embodiment 4:
1. obtain solution process reference example in 1. 1., 2. step, but oxalic acid solution concentration is increased to 0.5mol/L;
2. solution A and nickel foam are added in the there-necked flask, with the heating of back flow reaction stove up to temperature stabilization at 100 ℃, the while stirs with Reasonable Speed;
3. oxalic acid solution is dripped in the entering flask, and reacted 1 hour down at 100 ℃;
4. calcining manners is with 1. identical.
This method can be accomplished reaction owing to improved the temperature of back flow reaction in shorter time, but higher temperature has certain influence to the excellent pattern of zinc cobalt oxide nano.And because oxalic acid is that assurance is excessive in reaction, so concentration change within the specific limits can not influence reaction result.
Embodiment 5:
1. 4. 3. 2. 1. reaction raw materials preparation and back flow reaction process and embodiment go on foot in 1. identical.
2. the nickel foam sheet that makes is placed on calcination in the Muffle furnace, compares in 1. with embodiment, the temperature of calcination is risen to 500 ℃, annealing time also was made as 120 minutes.Natural cooling obtains product afterwards.
1. this instance is compared with embodiment, because calcination time prolongs, temperature improves, thus the degree of crystallinity of zinc cobalt oxide nano rod increase to some extent, and with the nickel foam substrate combine also more tight, but the pattern that lacks the part nanometer rods can be damaged.
After obtaining cobalt acid zinc nanometer rods/nickel foam combination electrode, the present invention forms three electrode super capacitor test systems with kind electrode as the work electrode and conventional reference electrode (platinum electrode), the reference electrode (mercury/mercury oxide) of new structure together.And adopt 1 mole every liter potassium hydroxide solution as electrolyte.The results of property of the ultracapacitor that obtains after the test is illustrated in the middle of the accompanying drawing 4,5,6.As can be seen from Figure 4, this kind cobalt acid zinc nanometer rods/nickel foam combination electrode circulates under the electric current of 2A/g and still maintains the capacity up to 1200F/g after 1000 times, this be existing super capacitor material inaccessiable.And in high electric current (6A/g) charge-discharge test, find that kind electrode can also remain on the high-capacitance of 1000F/g, the cyclical stability of visible cobalt acid zinc nanometer rods/nickel foam combination electrode is very outstanding, has guaranteed useful life.Fig. 5 has explained the increase along with charging current; The specific capacity of ultracapacitor keeps a metastable scope basically; This highlights the high magnification character that cobalt acid zinc nanometer rods/the nickel foam combination electrode is very good, this be after the characteristic of the special needs of batteries of electric automobile institute.Fig. 6 has shown that this kind capacitor has up to the energy density of 31Wh/kg and the power density of 20kW/kg.
The present invention not only is confined to above-mentioned embodiment; Persons skilled in the art are according to content disclosed by the invention; Can adopt other multiple embodiment embodiment of the present invention, therefore, every employing project organization of the present invention and thinking; Do some simple designs that change or change, all fall into the scope of the present invention's protection.
Claims (5)
1. cobalt acid zinc nanometer rods/nickel foam combination electrode is characterized in that, growth has cobalt acid zinc nanometer rods on the nickel foam sheet.
2. method for preparing cobalt acid zinc nanometer rods/nickel foam combination electrode; Be specially: the nickel foam sheet is immersed in the mixed solution of zinc nitrate and cobalt nitrate; Insulation after being heated to 80 °~100 ℃ drips oxalic acid solution, and reaction grows the nanostructure presoma on nickel foam; The taking-up nickel foam is cleaned successively, is dried and calcining obtains cobalt acid zinc nanometer rods/nickel foam combination electrode.
3. the method for preparing cobalt acid zinc nanometer rods/nickel foam combination electrode according to claim 2 is characterized in that the concentration of said zinc nitrate and cobalt nitrate is respectively 0.017~0.034mol/L and 0.033~0.066mol/L.
4. the method for preparing cobalt acid zinc nanometer rods/nickel foam combination electrode according to claim 2 is characterized in that, is incubated 1-2 hour.
5. the said cobalt acid of the claim zinc nanometer rods/application of nickel foam combination electrode in ultracapacitor is characterized in that, with its work electrode as ultracapacitor.
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Cited By (16)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103420431A (en) * | 2013-07-31 | 2013-12-04 | 上海理工大学 | Preparation method ofzinc cobaltatenanometer material doped with zinc oxide |
CN103440998A (en) * | 2013-08-21 | 2013-12-11 | 吉林大学 | Zinc cobaltate nanosheet array/foamed nickel combined electrode, preparation method and application thereof |
CN103956483A (en) * | 2014-04-30 | 2014-07-30 | 新疆维吾尔自治区产品质量监督检验研究院 | Preparation method and application of zinc cobaltate/nickel oxide core-shell nanowire array |
CN104310492A (en) * | 2014-09-29 | 2015-01-28 | 安徽工业大学 | Neodymium cobalt oxide nanorod and preparation method thereof |
CN104310493A (en) * | 2014-09-29 | 2015-01-28 | 安徽工业大学 | Dysprosium cobalt oxide nanorod and preparation method thereof |
CN104402066A (en) * | 2014-09-29 | 2015-03-11 | 安徽工业大学 | Terbium cobalt oxide nano rod and preparation method thereof |
CN105244192A (en) * | 2015-10-27 | 2016-01-13 | 渤海大学 | Magnesium cobaltite porous nanowire array/ nickel foam composite electrode material preparation method |
CN105336503A (en) * | 2015-11-27 | 2016-02-17 | 渤海大学 | Preparation method of copper cobaltate porous microrod and nickel foam composite electrode material |
CN105355467A (en) * | 2015-11-27 | 2016-02-24 | 渤海大学 | Preparation method of magnesium cobaltate porous micro-rod/ foamed nickel combined electrode material |
CN105390298A (en) * | 2015-12-11 | 2016-03-09 | 中航锂电(洛阳)有限公司 | Lithium ion capacitor negative unit, cell and lithium ion capacitor |
CN105895388A (en) * | 2016-06-18 | 2016-08-24 | 合肥松雷信息科技有限公司 | Preparation method for three-dimensional porous sheet-shaped zinc cobaltate nanomaterial |
CN106340403A (en) * | 2016-09-30 | 2017-01-18 | 江苏大学 | Preparation method and purpose of zinc cobaltate nano wire or nanometer band electrode material |
CN107032414A (en) * | 2017-03-13 | 2017-08-11 | 中山大学 | A kind of preparation method of the sour zinc nano-material of flexible cobalt |
CN107275105A (en) * | 2017-08-04 | 2017-10-20 | 南京理工大学 | Electrode material for super capacitor and preparation method thereof |
CN109599564A (en) * | 2018-11-27 | 2019-04-09 | 东华大学 | Cobalt acid nickel array self-supporting large area air electrode and its preparation and application |
CN109850955B (en) * | 2019-03-19 | 2021-10-12 | 合肥国轩高科动力能源有限公司 | Negative electrode material ZnCo of lithium ion battery2O4Method for preparing nano-rod |
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CN103420431B (en) * | 2013-07-31 | 2014-10-08 | 上海理工大学 | Preparation method ofzinc cobaltatenanometer material doped with zinc oxide |
CN103420431A (en) * | 2013-07-31 | 2013-12-04 | 上海理工大学 | Preparation method ofzinc cobaltatenanometer material doped with zinc oxide |
CN103440998A (en) * | 2013-08-21 | 2013-12-11 | 吉林大学 | Zinc cobaltate nanosheet array/foamed nickel combined electrode, preparation method and application thereof |
CN103440998B (en) * | 2013-08-21 | 2016-05-04 | 吉林大学 | A kind of cobalt acid zinc nanometer sheet array/nickel foam combination electrode, preparation method and application thereof |
CN103956483B (en) * | 2014-04-30 | 2016-01-13 | 新疆维吾尔自治区产品质量监督检验研究院 | The preparation method and application of cobalt acid zinc/nickel oxide core-shell nano linear array |
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CN104402066A (en) * | 2014-09-29 | 2015-03-11 | 安徽工业大学 | Terbium cobalt oxide nano rod and preparation method thereof |
CN104310493A (en) * | 2014-09-29 | 2015-01-28 | 安徽工业大学 | Dysprosium cobalt oxide nanorod and preparation method thereof |
CN104310492B (en) * | 2014-09-29 | 2016-03-30 | 安徽工业大学 | A kind of neodymium cobalt/cobalt oxide nanometer rod and preparation method thereof |
CN104310492A (en) * | 2014-09-29 | 2015-01-28 | 安徽工业大学 | Neodymium cobalt oxide nanorod and preparation method thereof |
CN104402066B (en) * | 2014-09-29 | 2016-05-11 | 安徽工业大学 | A kind of terbium cobalt/cobalt oxide nanometer rods and preparation method thereof |
CN105244192A (en) * | 2015-10-27 | 2016-01-13 | 渤海大学 | Magnesium cobaltite porous nanowire array/ nickel foam composite electrode material preparation method |
CN105336503B (en) * | 2015-11-27 | 2018-06-01 | 渤海大学 | A kind of preparation method of cobalt acid copper multi-pore micron stick/nickel foam combination electrode material |
CN105336503A (en) * | 2015-11-27 | 2016-02-17 | 渤海大学 | Preparation method of copper cobaltate porous microrod and nickel foam composite electrode material |
CN105355467A (en) * | 2015-11-27 | 2016-02-24 | 渤海大学 | Preparation method of magnesium cobaltate porous micro-rod/ foamed nickel combined electrode material |
CN105390298A (en) * | 2015-12-11 | 2016-03-09 | 中航锂电(洛阳)有限公司 | Lithium ion capacitor negative unit, cell and lithium ion capacitor |
CN105895388A (en) * | 2016-06-18 | 2016-08-24 | 合肥松雷信息科技有限公司 | Preparation method for three-dimensional porous sheet-shaped zinc cobaltate nanomaterial |
CN106340403A (en) * | 2016-09-30 | 2017-01-18 | 江苏大学 | Preparation method and purpose of zinc cobaltate nano wire or nanometer band electrode material |
CN107032414A (en) * | 2017-03-13 | 2017-08-11 | 中山大学 | A kind of preparation method of the sour zinc nano-material of flexible cobalt |
CN107032414B (en) * | 2017-03-13 | 2019-04-23 | 中山大学 | A kind of preparation method of flexibility cobalt acid zinc nano-material |
CN107275105A (en) * | 2017-08-04 | 2017-10-20 | 南京理工大学 | Electrode material for super capacitor and preparation method thereof |
CN107275105B (en) * | 2017-08-04 | 2019-01-15 | 南京理工大学 | Electrode material for super capacitor and preparation method thereof |
CN109599564A (en) * | 2018-11-27 | 2019-04-09 | 东华大学 | Cobalt acid nickel array self-supporting large area air electrode and its preparation and application |
CN109599564B (en) * | 2018-11-27 | 2022-09-06 | 东华大学 | Nickel cobaltate array self-supporting large-area air electrode and preparation and application thereof |
CN109850955B (en) * | 2019-03-19 | 2021-10-12 | 合肥国轩高科动力能源有限公司 | Negative electrode material ZnCo of lithium ion battery2O4Method for preparing nano-rod |
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