CN103700512A - ZnMn2O4 electrode material and preparation method thereof - Google Patents
ZnMn2O4 electrode material and preparation method thereof Download PDFInfo
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- CN103700512A CN103700512A CN201310628793.7A CN201310628793A CN103700512A CN 103700512 A CN103700512 A CN 103700512A CN 201310628793 A CN201310628793 A CN 201310628793A CN 103700512 A CN103700512 A CN 103700512A
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- electrode material
- znmn
- electrode
- znmn2o4
- citric acid
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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 ZnMn2O4 electrode material, and a preparation method and an application of the ZnMn2O4 electrode material. The ZnMn2O4 electrode material is characterized by being prepared by the following raw materials: manganous nitrate, zinc nitrate, citric acid and cetyl trimethyl ammonium bromide (CTAB) at a mole ratio of (2.3-1.8):(1.2-0.8):(1.3-0.8):(1.2-0.7). The ZnMn2O4 material is prepared by a solvothermal method which is simple, convenient and quick to operate, has the advantages of high specific capacitance and good cycling stability, and can be applied to an occasion of a high-stability and high-power density power supply due to the high specific capacitance and a stable working state of the material in an alkaline KOH (Potassium Oxide) electrolytic solution.
Description
Technical field
The present invention relates to a kind of electrode material and preparation method thereof.
Background technology
Ultracapacitor has the distinct advantages such as high power, long-life as a kind of novel energy storage unit, at the aspects such as hybrid power source system of consumption electronic product, UPS (uninterruptible power system) and electric vehicle, has broad application prospects.Ultracapacitor is according to the difference of energy storage mechanism, is divided into charcoal based super capacitor (double electric layer capacitor) and take the pseudo-capacitance capacitor that metal oxide and conducting polymer be electrode material.
In this two classes ultracapacitor, the ratio electric capacity of the active carbon that charcoal based super capacitor is used is lower, has limited the performance of ultracapacitor device.As everyone knows, the specific energy that improves energy storage device can alleviate the quality of himself, is applied to the weight that electric motor car can alleviate vehicle body, is therefore of great immediate significance.And the specific energy that will improve energy storage device will improve the ratio electric capacity of its crucial electrode material.The pseudo-capacitance capacitor that the metal oxide of take is electrode material just in time can meet above-mentioned requirements, and the ratio electric capacity of pseudo-capacitance oxide material can reach the several times of carbon electrode material, therefore becomes study hotspot both domestic and external.
In recent years in the metal oxide materials studied, RuO
2xH
2o is owing to maintaining the leading position up to 768F/g than electric capacity always, as the report of document [J.P.Zheng, J.Electrochem.Soc., 142 (1995): L6-L8.].Yet the shortcoming due to ruthenium with high price is difficult to commercialization.Therefore research direction is transferred to NiO gradually, as document [F.Zhang, Mater.Chem.Phys., 83 (2004): 260-264.], V
2o
5[H.Y.Lee, J.Solid State Chem., 148 (1999): 81-84.], MnO
2[Y.U.Jeong, J.Electrochem.Soc., 149 (2002): A1419-A1422.] and Co
3o
4the report of [Lin Cao, Yingke Zhou, Mei Lu, Hulin Li.Chinese Sci.Bulletin.48 (2003): 1212-1215] etc. comes up.MnO wherein
2due to cheap, the environmentally friendly extensive concern that is subject to domestic and international researcher.
Preparation method as the MnO2 of electrode material for super capacitor has: electrodeposition process, as report, the hydro thermal method of document [J.N.Broughton, Electrochimica Acta, 50 (2005): 4814-4819.], as document [V.Subramanian, J.Power Sources, 159 (2006): 361-364.] report, and coprecipitation, as document [M.Toupin, Chem.Mater., 14(2002) 3946-3952.] etc. report, its than electric capacity in 400F/g left and right.With RuO
2xH
2o compares, MnO
2ratio electric capacity need further raising.
It is reported MnO
2theory than electric capacity up to 1370F/g, as the report of document [Mathieu Toupin, Chem.Mater., 16 (2004): 3184-3190.].Researcher utilizes the good electrical conductivity [W.Zhou, H.Li and H.J.Fan, Chem.Commun.47 (2011) 3436. for J.Liu, C.Cheng] of zinc oxide; [G.R.Li, Z.L.Wang, F.L.Zheng, Y.N.Ou and Y.X.Tong, J.Mater.Chem.21 (2011) 4217.], prepared ZnO/MnO
2material improves it and compares electric capacity.
M.P.Yu etc. [M.P.Yu, H.T.Sun, X.Sun, F.Y.Lu, G.K.Wang, T.Hu, H.Qiu, JLian, Int.J.Electrochem.Sci., 8 (2013) 2313 – 2329.] adopt hydro thermal method to prepare ZnO/MnO
2electrode material.Structure and the pattern of core-shell material that adopted XRD, SETEM, XPS and Raman Characterization.Result shows, ZnO/MnO
2nucleocapsid structure has nano-scale structures, has formed high opening with porous nano surface topography and has had relative high degree of crystallinity.Electrochemical property test shows that sample has excellent invertibity and charge-discharge performance, ZnO/MnO
2nano material is at 1MNaSO
4in electrolyte, test, cyclic voltammetry shows that electrode has very high invertibity, ZnO/MnO in the potential range of 0-0.8V
2nano material reaches 151F/g than electric capacity when 10mV/s; When constant current density 2A/g, the ratio electric capacity of its material is still up to 210F/g.It is initial 97% that the ratio electric capacity (potential range be 0-0.8V) of electrode material after 2000 circulations remains, and has good cycle performance.
Xing Sun etc. [X.Sun, Q.Li, Y.N.Lu, Y.B.Mao.Chem.Commun., 49 (2013), 4456--4458] adopt hydro thermal method to prepare three-dimensional ZnO/MnO
2nucleocapsid structure electrode material.Adopt XRD, HRTEM, EDS, XPS and SEM to characterize structure and the pattern of composite material.Result shows, ZnO/MnO
2have nano-scale structures, under different temperatures roasting, material is also at nanoscale and have relatively high degree of crystallinity.Electrochemical property test shows that sample has excellent invertibity and charge-discharge performance, three-dimensional ZnO/MnO
2nucleocapsid structure is 300 ℃ of sintering temperatures, and cyclic voltammetry shows that electrode has very high invertibity, constant current density 0.02A/cm in the potential range of-0.2-0.6V
2time, the ratio electric capacity of its material is up to 31.299F/g.
And about research Zn-Mn composite metal oxide material ZnMn
2o
4be applied to the existing report of lithium battery aspect, as document [J.G.Kim, S.H.Lee, Y.Kim, W.B.Kim.Appl.Mater.Interfaces, 5 (2013) 1121-11328], [S.W.Kim, H.W.Lee, P.Muralidharan, Do.H.Seo, W.S.Yoon, D.K.Kim, K.Kang, Nano Res.4 (2011) 505 – 510].But ZnMn
2o
4material is applied to the electrode material of carrying high specific capacitance in ultracapacitor and has no at present report, therefore develops its Zn-Mn composite oxide of metal ZnMn
2o
4the new electrode material of high-performance super capacitor that material is carried high specific capacitance seems particularly important.
In sum, have no researchers both domestic and external Zn-Mn composition metal is applied to the report on ultracapacitor, therefore studying the preparation method that Zn-Mn material is new and improving it has very large researching value than electric capacity.
Summary of the invention
The object of the invention is to disclose a kind of ZnMn
2o
4electrode material and preparation method thereof, to meet the needs of association area development.
Described ZnMn
2o
4electrode material is to adopt the raw material of following mol ratio to prepare:
Manganese nitrate: zinc nitrate: citric acid: softex kw (CTAB)=2.3~1.8:1.2~0.8:1.3~0.8:1.2~0.7;
Preferably, be to adopt the raw material of following mol ratio to prepare: manganese nitrate: zinc nitrate: citric acid: softex kw (CTAB)=2:1:1:0.5;
Described ZnMn
2o
4electrode material is preparation method comprise the steps:
By manganese nitrate, zinc nitrate, citric acid and CTAB, add in ethanol, stir 1~3 hour, obtain the mixed solution that contains manganese nitrate, zinc nitrate, citric acid and CTAB;
In described mixed solution, the molar concentration of manganese nitrate is 3.0~5.0mmol/ml;
Then at 100~200 ℃, preferably descend heat treatment 24~72 hours, preferably 48 hours, can obtain described ZnMn
2o
4electrode material;
The ZnMn that adopts said method to obtain
2o
4electrode material, can be used for preparing electrode material for super capacitor.
Advantage of the present invention and good effect are: adopt simple to operate, solvent-thermal method is prepared ZnMn easily
2o
4material, first by ZnMn
2o
4material is applied in ultracapacitor, ZnMn
2o
4electrode material electrolyte ion in charge and discharge process embeds and deviates from mutually at its body, and the crystallinity of electrode material is lower, is more conducive to the embedding of ion and deviates from, and the utilance of material is just higher, thereby can improve its chemical property.The ZnMn that method of the present invention makes
2o
4material, first by ZnMn
2o
4material is applied in ultracapacitor, finds ZnMn
2o
4material has higher than electric capacity, the advantage of good cycling stability, and its high specific capacitance in alkaline KOH electrolyte and stable operating state, can be applicable to high stability, the occasion of high-power density power supply.
Accompanying drawing explanation
Fig. 1 is the prepared ZnMn of different solvents thermal response temperature
2o
4electrode material XRD figure, sample is called T-120, T-140, T-160, T-180 and T-200 are respectively at 120 ℃, and 140 ℃, 160 ℃, the sample preparing at the solvent heat temperature of 180 ℃ and 200 ℃.
Fig. 2 is the prepared ZnMn of different solvents thermal response temperature
2o
4electrode material SEM figure.
Wherein: a is the sample preparing at the solvent heat temperature of 120 ℃, b is the sample preparing at the solvent heat temperature of 140 ℃, and c is the sample preparing at the solvent heat temperature of 160 ℃, and d is the sample preparing at the solvent heat temperature of 180 ℃; E is the sample preparing at the solvent heat temperature of 200 ℃.
Fig. 3 is the prepared ZnMn of different solvents thermal response temperature
2o
4the cyclic voltammetry curve figure of electrode material when sweep speed is 5mV/s, material has good electrochemical reversibility.
Fig. 4 is the prepared ZnMn of different solvents thermal response temperature
2o
4the ratio electric capacity of electrode material when sweep speed is 5mV/s.
Fig. 5 is 180 ℃ of prepared ZnMn of solvent thermal reaction temperature
2o
4the circulation volt figure of electrode material under different scanning rates.
Fig. 6 is 180 ℃ of prepared ZnMn of solvent thermal reaction temperature
2o
4the constant current charge-discharge curve chart of electrode material, has obvious fake capacitance charge-discharge performance.
Fig. 7 is 180 ℃ of prepared ZnMn of solvent thermal reaction temperature
2o
4the electrochemical impedance spectrogram of electrode material, its impedance is little, is suitable as electrode material for super capacitor.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail, but the present embodiment is not limited to the present invention, every employing similarity method of the present invention and similar variation thereof, all should list protection scope of the present invention in.
Embodiment 1
ZnMn
2o
4the preparation of electrode material
Adopt solvent-thermal method, by 2.0mmol manganese nitrate, 1.0mmol zinc nitrate, 1.0mmol citric acid, 0.5mmolCTAB, joins in the absolute ethyl alcohol of 35ml, stirs about 3 hours to forming colourless transparent solution; Pour mixed solution into hydrothermal reaction kettle, solvent heat treatment reaction 48 hours, obtains target product: ZnMn
2o
4material.
Solvent thermal reaction temperature is 120 ℃.
Adopt three-electrode system to carry out cyclic voltammetry, respectively with 3 * 5cm
2the platinized platinum of size and saturated calomel electrode (SCE) are as auxiliary electrode and reference electrode, ZnMn
2o
4material is as work electrode, and test macro is CHI660C electrochemical workstation.Sweep speed is 5mV/s, and potential region is-0.1~0.7V.Electrolyte is the KOH electrolyte of 2M.
Electrochemical property test result shows, ZnMn
2o
4the ratio electric capacity of material is 72F/g.
Embodiment 2
Press described in embodiment 1, adopt solvent-thermal method, by 2.0mmol manganese nitrate, 1.0mmol zinc nitrate, 1.0mmol citric acid, 0.5mmolCTAB, joins in the absolute ethyl alcohol of 35ml, stirs about 3 hours to forming colourless transparent solution; Pour mixed solution into hydrothermal reaction kettle, solvent heat treatment reaction 48 hours, obtains target product: ZnMn
2o
4material.Solvent thermal reaction temperature is 140 ℃.
Adopt three-electrode system to carry out cyclic voltammetry, respectively with 3 * 5cm
2the platinized platinum of size and saturated calomel electrode (SCE) are as auxiliary electrode and reference electrode, ZnMn
2o
4material is as work electrode, and test macro is CHI660C electrochemical workstation.Sweep speed is 5mV/s, and potential region is-0.1~0.7V.Electrolyte is the KOH aqueous solution of 2M.
Electrochemical property test result shows, ZnMn
2o
4the ratio electric capacity of material is 103F/g.
Embodiment 3
Press described in embodiment 1, adopt solvent-thermal method, by 2.0mmol manganese nitrate, 1.0mmol zinc nitrate, 1.0mmol citric acid, 0.5mmolCTAB, joins in the absolute ethyl alcohol of 35ml, stirs about 3 hours to forming colourless transparent solution; Pour mixed solution into hydrothermal reaction kettle, solvent heat treatment reaction 48 hours, obtains target product: ZnMn
2o
4material.Solvent thermal reaction temperature is 160 ℃.
Adopt three-electrode system to carry out cyclic voltammetry, respectively with 3 * 5cm
2the platinized platinum of size and saturated calomel electrode (SCE) are as auxiliary electrode and reference electrode, ZnMn
2o
4material is as work electrode, and test macro is CHI660C electrochemical workstation.Sweep speed is 5mV/s, and potential region is-0.1~0.7V.Electrolyte is the KOH aqueous solution of 2M.
Electrochemical property test result shows, ZnMn
2o
4the ratio electric capacity of material is 125F/g.
Embodiment 4
Press described in embodiment 1, adopt solvent-thermal method, by 2.0mmol manganese nitrate, 1.0mmol zinc nitrate, 1.0mmol citric acid, 0.5mmolCTAB, joins in the absolute ethyl alcohol of 35ml, stirs about 3 hours to forming colourless transparent solution; Pour mixed solution into hydrothermal reaction kettle, solvent heat treatment reaction 48 hours, obtains target product: ZnMn
2o
4material.Solvent thermal reaction temperature is 180 ℃.
Adopt three-electrode system to carry out cyclic voltammetry, respectively with 3 * 5cm
2the platinized platinum of size and saturated calomel electrode (SCE) are as auxiliary electrode and reference electrode, ZnMn
2o material is as work electrode, and test macro is CHI660C electrochemical workstation.Sweep speed is 5mV/s, and potential region is-0.1~0.7V.Electrolyte is the KOH aqueous solution of 2M.
Electrochemical property test result shows, ZnMn
2o
4the ratio electric capacity of material is 129F/g.
Press described in embodiment 1, adopt solvent-thermal method, by 2.0mmol manganese nitrate, 1.0mmol zinc nitrate, 1.0mmol citric acid, 0.5mmolCTAB, joins in the absolute ethyl alcohol of 35ml, stirs about 3 hours to forming colourless transparent solution; Pour mixed solution into hydrothermal reaction kettle, solvent heat treatment reaction 48 hours, obtains target product: ZnMn
2o
4material.Solvent thermal reaction temperature is 120 ℃.
Adopt three-electrode system to carry out cyclic voltammetry, respectively with 3 * 5cm
2the platinized platinum of size and saturated calomel electrode (SCE) are as auxiliary electrode and reference electrode, ZnMn
2o
4nano material is as work electrode, and test macro is CHI660C electrochemical workstation.Sweep speed is 5mV/s, and potential region is-0.1~0.7V.Electrolyte is the KOH aqueous solution of 2M.
Electrochemical property test result shows, ZnMn
2o
4the ratio electric capacity of material is 124F/g.
Figure at different solvents thermal response temperature: XRD figure is shown in Fig. 1; SEM figure is shown in Fig. 2; Different solvents hot temperature degree cyclic voltammogram is shown in Fig. 3; Different solvents hot temperature is shown in Fig. 4 at the cyclic voltammogram of sweep speed 5mV/s; 180 ℃ of the solvent heat temperature cyclic voltammogram under different scanning rates is shown in Fig. 5; The electrograph that charges and discharge that solvent heat temperature is 180 ℃ is shown in Fig. 6; 180 ℃ of chemical impedance spectrograms of solvent heat temperature are shown in Fig. 7.
Claims (6)
1.ZnMn
2o
4electrode material, is characterized in that, is to adopt the raw material of following mol ratio to prepare:
Manganese nitrate: zinc nitrate: citric acid: softex kw (CTAB)=2.3~1.8:1.2~0.8:1.3~0.8:1.2~0.7.
2. ZnMn according to claim 1
2o
4electrode material, is characterized in that, is to adopt the raw material of following mol ratio to prepare: manganese nitrate: zinc nitrate: citric acid: softex kw (CTAB)=2:1:1:0.5.
3. ZnMn according to claim 1 and 2
2o
4the preparation method of electrode material, is characterized in that, comprises the steps:
By manganese nitrate, zinc nitrate, citric acid and CTAB, add in ethanol, stir, obtain the mixed solution that contains manganese nitrate, zinc nitrate, citric acid and CTAB; Then heat treatment, can obtain described ZnMn
2o
4electrode material.
4. method according to claim 3, is characterized in that, in described mixed solution, the molar concentration of manganese nitrate is 3.0~5.0mmol/ml.
5. method according to claim 3, is characterized in that, 100~200 ℃ of solvent heat treatment 24~72 hours.
6. ZnMn according to claim 1 and 2
2o
4the application of electrode material, is characterized in that, for the preparation of electrode material for super capacitor.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108306059A (en) * | 2018-02-01 | 2018-07-20 | 吉首大学 | The preparation method of environmentally protective high power water system Zinc ion battery |
CN108467066A (en) * | 2018-04-08 | 2018-08-31 | 淮北师范大学 | A kind of porous micro-nano structure ZnMn of rice-shaped2O4Lithium ion battery negative material |
CN110474017A (en) * | 2019-08-29 | 2019-11-19 | 瑞海泊有限公司 | The preparation method and applications of mangaic acid zinc electrode |
CN110492100A (en) * | 2019-09-02 | 2019-11-22 | 吉林大学 | Zinc manganate nanoparticle carbon cloth composite material and preparation method thereof and lithium ion battery |
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2013
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CN101274779A (en) * | 2008-05-14 | 2008-10-01 | 华中师范大学 | Nano-scaled materials ZnMn2O4 for lithium storage and preparation thereof |
US20130115513A1 (en) * | 2011-11-07 | 2013-05-09 | Samsung Corning Precision Materials Co., Ltd. | Electrode active material, preparation method thereof, and electrode and lithium battery containing the same |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108306059A (en) * | 2018-02-01 | 2018-07-20 | 吉首大学 | The preparation method of environmentally protective high power water system Zinc ion battery |
CN108467066A (en) * | 2018-04-08 | 2018-08-31 | 淮北师范大学 | A kind of porous micro-nano structure ZnMn of rice-shaped2O4Lithium ion battery negative material |
CN110474017A (en) * | 2019-08-29 | 2019-11-19 | 瑞海泊有限公司 | The preparation method and applications of mangaic acid zinc electrode |
CN110492100A (en) * | 2019-09-02 | 2019-11-22 | 吉林大学 | Zinc manganate nanoparticle carbon cloth composite material and preparation method thereof and lithium ion battery |
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Application publication date: 20140402 |