CN102903534A - Method for preparing super capacitor material with Co3O4-Au-MnO2 three-dimensional hierarchical heterogeneous nanosheet array - Google Patents

Method for preparing super capacitor material with Co3O4-Au-MnO2 three-dimensional hierarchical heterogeneous nanosheet array Download PDF

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CN102903534A
CN102903534A CN2012104400362A CN201210440036A CN102903534A CN 102903534 A CN102903534 A CN 102903534A CN 2012104400362 A CN2012104400362 A CN 2012104400362A CN 201210440036 A CN201210440036 A CN 201210440036A CN 102903534 A CN102903534 A CN 102903534A
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chip arrays
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super capacitor
capacitor material
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CN102903534B (en
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胡俊青
李文尧
邹儒佳
李高
徐开兵
孙彦刚
王滕
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Donghua University
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Abstract

The invention relates to a method for preparing a super capacitor material with a Co3O4-Au-MnO2 three-dimensional hierarchical heterogeneous nanosheet array. The method comprises the following steps of; (1) preparing a Co3O4 nanosheet array of a precursor; (2) evaporating the surface of the Co3O4 nanosheet array by using a plasma sputtering method, and thus obtaining an Au-film-covered Co3O4 nanosheet array; and (3) electrochemically depositing the Au-film-covered Co3O4 nanosheet array under the condition of potential of 0.9 V, coating MnO2 on the surface of the Au-film-covered Co3O4 nanosheet array, cleaning, drying and roasting a reaction product, and thus obtaining the super capacitor material. The method is easy to operate, and complicated equipment is eliminated. A Co3O4-Au-MnO2 nanosheet array which is prepared by using the method is uniformly distributed, has a three-dimensional hierarchical hetero-structure, and is high in electrochemical performance and wide in application prospect.

Description

Co 3O 4-Au-MnO 2The preparation method of the heterogeneous nano-chip arrays super capacitor material of three-dimensional classification
Technical field
The invention belongs to the preparation field of super capacitor material, particularly a kind of Co 3O 4-Au-MnO 2The preparation method of the heterogeneous nano-chip arrays super capacitor material of three-dimensional classification.
Background technology
As everyone knows, the energy is the material base of human survival and development, and facing mankind serious energy crisis at present.The energy saver of research and development energy storage and recovery is one of effective way that solves energy problem.Electrochemical capacitor is as a kind of novel energy-storing device, have than the much bigger energy density of traditional capacitor and the power density more much higher than battery, the advantage such as the energy collecting metric density is high, power density is high, have extended cycle life, the charging interval is short and storage period is long.At aspects such as automobile, electric power, railway, communication, national defence, consumer electronic product huge using value and market potential are arranged, caused domestic and international scientist's broad interest.The electrode material that is widely used at present ultracapacitor has porous carbon material, transition metal oxide and conducting polymer (P.Simon et al, Nat.Mater.2008,7,845.).
In these materials, cobaltosic oxide and manganese dioxide in the transition metal oxide are considered to the most attractive selection, because that it has is cheap, environmental friendliness and superior capacitive property, have caused the extensive concern of vast researcher.The cobaltosic oxide of present various patterns and manganese oxide material all are produced, and method is various, for example chemical precipitation method, solid phase method, sol-gal process etc. (R.B.Rakhi et al, Nano Lett.2012,12,2559.).Yet the low electric conductivity of Mn oxide has limited its application aspect high-performance super capacitor.In order to improve desired properties, the preparation of metals composite construction nano material of introducing excellent electric conductivity has caused scientist's research interest gradually.
Existing human complicated approach with Au as conductive layer deposition MnO 2Prepared WO 3-x-Au-MnO 2Composite material, but still be not enough to meet the need of market than electric capacity.
Therefore, need a kind of simply and easily method of development, prepare eco-friendly, as to have excellent properties multi-element transition metal oxides super capacitor material.
Summary of the invention
Technical problem to be solved by this invention provides a kind of Co 3O 4-Au-MnO 2The preparation method of the heterogeneous nano-chip arrays super capacitor material of three-dimensional classification, the method is simple to operate, does not need special installation, the Co of prepared three-dimensional classification heterostructure, chemical property excellence 3O 4-Au-MnO 2Nano-chip arrays is evenly distributed.
A kind of Co of the present invention 3O 4-Au-MnO 2The preparation method of the heterogeneous nano-chip arrays super capacitor material of three-dimensional classification comprises:
(1) nickel foam is being contained the Co (NO of DMSO 3) 2In the aqueous solution under-1V current potential electrochemical deposition prepare Co (OH) 2Nano-chip arrays, then calcining obtains presoma Co 3O 4Nano-chip arrays;
(2) utilize plasma sputtering at above-mentioned Co 3O 4The surperficial evaporation of nano-chip arrays forms the film that the layer of Au particle forms, and obtains the Co that the Au film covers 3O 4Nano-chip arrays;
(3) Co that above-mentioned Au film is covered 3O 4Nano-chip arrays places the Mn (CH that contains DMSO 3COO) 2And CH 3COONH 4Mixed aqueous solution in, electrochemical deposition under the 0.9V current potential then is with MnO 2Be coated on the Co that the Au film covers 3O 4The surface of nano-chip arrays; After reaction was finished, with dry after the product cleaning that obtains, calcining namely got Co at last 3O 4-Au-MnO 2The heterogeneous nano-chip arrays super capacitor material of three-dimensional classification.
Calcining described in the step (1) is for to calcine in Muffle furnace.
The Co (NO that contains DMSO described in the step (1) 3) 2Co (NO in the aqueous solution 3) 2Concentration be 0.01 ~ 0.05mol/L.
The time of the evaporation described in the step (2) is 0.5 ~ 3min.
The Mn (CH that contains DMSO described in the step (3) 3COO) 2And CH 3COONH 4Mixed aqueous solution in Mn (CH 3COO) 2Concentration be 0.005 ~ 0.02mol/L, CH 3COONH 4Concentration be 0.01 ~ 0.05mol/L.
Cleaning described in the step (3) is for using respectively ethanol, washed with de-ionized water 1-3 time.
Drying described in the step (3) is in 60-80 ℃ of dry 3-5h.
Calcining described in the step (3) is for calcining 2h. in Muffle furnace
The Co that the present invention obtains 3O 4-Au-MnO 2Material is the three-dimensional classification heterostructure of nanometer.
The concrete behaviour of the plasma sputtering that adopts among the present invention is: (1) puts into the target groove with gold target, will need the surface-treated sample to place on the rotary sample platform, and closed sample stage rotary switch covers cloche; (2) open mechanical pump, with vacustat at 7-10Pa, closed ion current switch, rotation high pressure knob is regulated high pressure, makes in the experimentation current stabilization at 10mA; Close high pressure when (3) sedimentation time finishes, disconnect the ion current switch, open at last the inflation knob and make the cloche internal pressure return to atmospheric pressure, take out at last sample.
The present invention utilizes the precursor synthesis array type sheet Co for preparing under the different condition under the electrochemical deposition technique condition 3O 4-Au-MnO 2Nano material, the preparation structure is unique, the excellent Co of chemical property 3O 4-Au-MnO 2The heterogeneous nano-chip arrays of three-dimensional classification.
The present invention take common mineral solution as raw material, by the experiment parameters such as concentration, time, temperature of reactant in the regulation and control electrochemical deposition process, prepares three-dimensional Co on the basis without follow-up use low-surface-energy material modified product surface 3O 4-Au-MnO 2Nano-chip arrays obtains the three-dimensional classification heterostructure that large tracts of land is evenly distributed, the Co of chemical property excellence 3O 4-Au-MnO 2Nano-chip arrays.
The present invention passes through simple electrochemical deposition technique, the three-dimensional classification heterostructure that success is synthetic, the Co of chemical property excellence 3O 4-Au-MnO 2Nano-chip arrays will explored the technology of preparing of new electrode materials, screening more preferably, the electrode material of high specific capacitance or volume energy density, high charge-discharge power density, improve the performance of electrochemical capacitor, solve the energy scarcity aspect and contribute.
The present invention has synthesized Co by electrochemical deposition and plasma sputtering technology 3O 4-Au-MnO 2The heterogeneous nano-chip arrays of three-dimensional classification, the Co of preparation 3O 4-Au-MnO 2The heterogeneous nano-chip arrays of three-dimensional classification has good electrochemical stability, and circulating does not have capacitance loss 5000 times substantially.Because the product of preparation is evenly distributed, pattern is regular, and just can obtain the material of three-dimensional classification heterostructure, chemical property excellence by simple synthetic method.Therefore, the Co of the present invention's preparation 3O 4-Au-MnO 2The heterogeneous nano-chip arrays of three-dimensional classification has huge application potential at aspects such as ultracapacitor, lithium ion battery materials.
Beneficial effect;
(1) preparation method of the present invention is simple to operate, does not need special installation;
(2) the prepared Co of the present invention 3O 4-Au-MnO 2Nano-chip arrays is evenly distributed, and is three-dimensional classification heterostructure, and chemical property is excellent, can greatly expand electrochemical capacitor material preparation method and application.
Description of drawings
Fig. 1 is the heterogeneous Co of three-dimensional classification that the present invention prepares 3O 4-Au-MnO 2The ESEM picture of nano-chip arrays;
Fig. 2 is the heterogeneous Co of three-dimensional classification that the present invention prepares 3O 4-Au-MnO 2The XPS picture of nano-chip arrays;
Fig. 3 is the heterogeneous Co of three-dimensional classification that the present invention prepares 3O 4-Au-MnO 2The cyclical stability test picture of nano-chip arrays.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
The present invention adopts electrochemical deposition technique, by allocating specific reaction solution, will be immersed in the reaction solution as work electrode through the nickel foam of removing surface oxide layer, and deposition obtains Co 3O 4Evaporation Au film behind the presoma, electrochemical deposition certain hour in another solution then, the Co of preparation chemical property excellence 3O 4-Au-MnO 2The heterogeneous nano-chip arrays of three-dimensional classification.
Embodiment 1
(1) utilize nickel foam containing the 1%(volumetric concentration) Co (NO of the 0.02mol/L of DMSO 3) 2In the aqueous solution under-1V electrochemical deposition prepare Co (OH) 2Nano-chip arrays, then 250 ℃ of lower calcining 2h in Muffle furnace obtain black Co 3O 4Nano-chip arrays;
(2) the recycling plasma sputtering is at the Co of acquisition 3O 4Nanometer sheet surface evaporation 0.5min obtains the Co that the Au film covers 3O 4The nano-chip arrays presoma;
(3) above-mentioned presoma is placed contain the 1%(volumetric concentration) the 0.005mol/L Mn (CH of DMSO 3COO) 2With 0.01mol/L CH 3COONH 4Mixed aqueous solution in, then use electrochemical deposition method at Co 3O 4Then-Au nanometer sheet surface potentiostatic electrodeposition 2min under the 0.9V current potential uses product respectively ethanol, deionized water rinsing for several times, 60-80 ℃, dry 3-5h, and then 200 ℃ of lower calcining 2h in Muffle furnace obtain Co 3O 4-Au-MnO 2The heterogeneous nano-chip arrays of three-dimensional classification.
Embodiment 2
(1) utilize nickel foam containing the 3%(volumetric concentration) Co (NO of the 0.03mol/L of DMSO 3) 2In the aqueous solution-1V under electrochemical deposition prepare Co (OH) 2Nano-chip arrays, then 250 ℃ of lower calcining 2h in Muffle furnace obtain black Co 3O 4Nano-chip arrays;
(2) the recycling plasma sputtering is at the Co of acquisition 3O 4Nanometer sheet surface evaporation 1min obtains the Co that the Au film covers 3O 4The nano-chip arrays presoma;
(3) above-mentioned presoma is placed contain the 5%(volumetric concentration) the 0.01mol/L Mn (CH of DMSO 3COO) 2With 0.02mol/L CH 3COONH 4Mixed aqueous solution in, then use electrochemical deposition method at Co 3O 4Then-Au nanometer sheet surface potentiostatic electrodeposition 5min under the 0.9V current potential uses product respectively ethanol, deionized water rinsing for several times, 60-80 ℃, dry 3-5h, and then 200 ℃ of lower calcining 2h in Muffle furnace obtain Co 3O 4-Au-MnO 2The heterogeneous nano-chip arrays of three-dimensional classification.
Embodiment 3
Utilize nickel foam containing the 5%(volumetric concentration) Co (NO of the 0.05mol/L of DMSO 3) 2In the aqueous solution-1V under electrochemical deposition prepare Co (OH) 2Nano-chip arrays, then 250 ℃ of lower calcining 2h in Muffle furnace obtain black Co 3O 4Nano-chip arrays;
The Co that the recycling plasma sputtering is obtaining 3O 4Nanometer sheet surface evaporation 1.5min obtains the Co that the Au film covers 3O 4The nano-chip arrays presoma;
Above-mentioned presoma placed contains the 10%(volumetric concentration) the 0.005mol/L Mn (CH of DMSO 3COO) 2With 0.02mol/L CH 3COONH 4Mixed aqueous solution in, then use electrochemical deposition method at Co 3O 4Then-Au nanometer sheet surface potentiostatic electrodeposition 10min under the 0.9V current potential uses product respectively ethanol, deionized water rinsing for several times, 60-80 ℃, dry 3-5h, and then 200 ℃ of lower calcining 2h in Muffle furnace obtain Co 3O 4-Au-MnO 2The heterogeneous nano-chip arrays of three-dimensional classification.
Embodiment 4
(1) utilize nickel foam containing the 2%(volumetric concentration) Co (NO of the 0.02mol/L of DMSO 3) 2In the aqueous solution-1V under electrochemical deposition prepare Co (OH) 2Nano-chip arrays, then 250 ℃ of lower calcining 2h in Muffle furnace obtain black Co 3O 4Nano-chip arrays;
(2) the recycling plasma sputtering is at the Co of acquisition 3O 4Nanometer sheet surface evaporation 3min obtains the Co that the Au film covers 3O 4The nano-chip arrays presoma;
(3) above-mentioned presoma is placed contain the 5%(volumetric concentration) the 0.02mol/L Mn (CH of DMSO 3COO) 2With 0.05mol/L CH 3COONH 4Mixed aqueous solution in, then use electrochemical deposition method at Co 3O 4Then-Au nanometer sheet surface potentiostatic electrodeposition 20min under the 0.9V current potential uses product respectively ethanol, deionized water rinsing for several times, 60-80 ℃, dry 3-5h, and then 200 ℃ of lower calcining 2h in Muffle furnace obtain Co 3O 4-Au-MnO 2The heterogeneous nano-chip arrays of three-dimensional classification.

Claims (8)

1. Co 3O 4-Au-MnO 2The preparation method of the heterogeneous nano-chip arrays super capacitor material of three-dimensional classification comprises:
(1) nickel foam is being contained the Co (NO of DMSO 3) 2In the aqueous solution under-1V current potential electrochemical deposition prepare Co (OH) 2Nano-chip arrays, then calcining obtains presoma Co 3O 4Nano-chip arrays;
(2) utilize plasma sputtering at above-mentioned Co 3O 4The surperficial evaporation of nano-chip arrays forms the film that the layer of Au particle forms, and obtains the Co that the Au film covers 3O 4Nano-chip arrays;
(3) Co that above-mentioned Au film is covered 3O 4Nano-chip arrays places the Mn (CH that contains DMSO 3COO) 2And CH 3COONH 4Mixed aqueous solution in, electrochemical deposition under the 0.9V current potential then is with MnO 2Be coated on the Co that the Au film covers 3O 4The surface of nano-chip arrays; After reaction is finished, with dry after the product cleaning that obtains, at last calcining, and get final product.
2. a kind of Co according to claim 1 3O 4-Au-MnO 2The preparation method of the heterogeneous nano-chip arrays super capacitor material of three-dimensional classification, it is characterized in that: the calcining described in the step (1) is for to calcine in Muffle furnace.
3. a kind of Co according to claim 1 3O 4-Au-MnO 2The preparation method of the heterogeneous nano-chip arrays super capacitor material of three-dimensional classification is characterized in that: the Co (NO that contains DMSO described in the step (1) 3) 2Co (NO in the aqueous solution 3) 2Concentration be 0.01 ~ 0.05mol/L.
4. a kind of Co according to claim 1 3O 4-Au-MnO 2The preparation method of the heterogeneous nano-chip arrays super capacitor material of three-dimensional classification, it is characterized in that: the time of the evaporation described in the step (2) is 0.5 ~ 3min.
5. a kind of Co according to claim 1 3O 4-Au-MnO 2The preparation method of the heterogeneous nano-chip arrays super capacitor material of three-dimensional classification is characterized in that: the Mn (CH that contains DMSO described in the step (3) 3COO) 2And CH 3COONH 4Mixed aqueous solution in Mn (CH 3COO) 2Concentration be 0.005 ~ 0.02mol/L, CH 3COONH 4Concentration be 0.01 ~ 0.05mol/L.
6. a kind of Co according to claim 1 3O 4-Au-MnO 2The preparation method of the heterogeneous nano-chip arrays super capacitor material of three-dimensional classification, it is characterized in that: the cleaning described in the step (3) is for using respectively ethanol, washed with de-ionized water 1-3 time.
7. a kind of Co according to claim 1 3O 4-Au-MnO 2The preparation method of the heterogeneous nano-chip arrays super capacitor material of three-dimensional classification is characterized in that: the drying described in the step (3) is in 60-80 ℃ of dry 3-5h.
8. a kind of Co according to claim 1 3O 4-Au-MnO 2The preparation method of the heterogeneous nano-chip arrays super capacitor material of three-dimensional classification is characterized in that: the calcining described in the step (3) is for calcining 2h in Muffle furnace.
CN201210440036.2A 2012-11-06 2012-11-06 Co 3o 4-Au-MnO 2the preparation method of the heterogeneous nano-chip arrays super capacitor material of three-dimensional classification Expired - Fee Related CN102903534B (en)

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Cited By (4)

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CN103500668A (en) * 2013-09-30 2014-01-08 武汉理工大学 MoO2/Co(OH)2 grading composite nano-material, and preparation method and application thereof
CN109205681A (en) * 2018-09-12 2019-01-15 嘉兴学院 A kind of three-dimensional hierarchical structure metal oxide and preparation method thereof
CN110223847A (en) * 2019-06-11 2019-09-10 江苏先创新能源有限公司 A kind of electrode material for super capacitor and preparation method
CN110993371A (en) * 2019-11-22 2020-04-10 南京理工大学 LiMnxOy@ C three-dimensional nanosheet array, preparation method and application thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103500668A (en) * 2013-09-30 2014-01-08 武汉理工大学 MoO2/Co(OH)2 grading composite nano-material, and preparation method and application thereof
CN103500668B (en) * 2013-09-30 2016-01-13 武汉理工大学 MoO 2/ Co (OH) 2classification composite nano materials and its preparation method and application
CN109205681A (en) * 2018-09-12 2019-01-15 嘉兴学院 A kind of three-dimensional hierarchical structure metal oxide and preparation method thereof
CN110223847A (en) * 2019-06-11 2019-09-10 江苏先创新能源有限公司 A kind of electrode material for super capacitor and preparation method
CN110993371A (en) * 2019-11-22 2020-04-10 南京理工大学 LiMnxOy@ C three-dimensional nanosheet array, preparation method and application thereof

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