CN101702375B - Preparation method of element doping manganese dioxide electrode material for super capacitor - Google Patents
Preparation method of element doping manganese dioxide electrode material for super capacitor Download PDFInfo
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- CN101702375B CN101702375B CN2009101865192A CN200910186519A CN101702375B CN 101702375 B CN101702375 B CN 101702375B CN 2009101865192 A CN2009101865192 A CN 2009101865192A CN 200910186519 A CN200910186519 A CN 200910186519A CN 101702375 B CN101702375 B CN 101702375B
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Abstract
The invention discloses a preparation method of an element doping manganese dioxide electrode material for a super capacitor, which is characterized by comprising the following steps: (1) synthesizing a LiAxMn2-xO4 powder material with a spinel structure by utilizing a suitable method, wherein A is selected from metallic addictive elements Ti, Ni, Sn, Co, Zn and Al, and x is within the range of 0.01-0.25%; and (2) utilizing lithium ion removal agent to remove lithium ions from the LiAxMn2-xO4 powder material obtained from step (1) under the condition of not destructing the spinel structure of a precursor, thereby obtaining the element-replacement MnO2-doping electrode material for the super capacitor. For the element doping manganese dioxide electrode material prepared by the invention, the Mn part in a lattice can be evenly replaced by doped elements, and the method has high industrial maturity and is a way with great potential for preparing the manganese dioxide electrode material for the super capacitor.
Description
Technical field
The invention belongs to the electrode material for super capacitor preparing technical field, be specifically related to the preparation method of a kind of ultracapacitor with element substitute doping manganese dioxide.
Background technology
Ultracapacitor (Supercapacitor) is a kind of novel energy-storing element between traditional capacitor and battery.It has the big and big advantage of rechargeable battery energy density of conventional capacitor power density concurrently, but the big electric current of abrupt release, but fast charging and discharging, and the charge efficiency height, recycle long, memory-less effect of life-span, basic Maintenance free in the use, environmentally safe has of crucial importance and wide application prospect at aspects such as mobile communication, information technology, industrial circle, consumer electronics, electric automobile, Aero-Space and science and techniques of defence in addition.
At present, the electrode material that is used for ultracapacitor mainly contains: carbon electrode material, metal oxide and hydrate electrode material thereof and conductive polymer electrodes material.Carbon electrode material mainly comes storage power based on the electric double layer principle, and is more relatively low than electric capacity;
Reversible fast n type, p type element doping mainly by taking place and going the redox reaction of mixing in conducting polymer materials in the polymer on the electrode, produce pseudo capacitance and come storage power, though it is higher than electric capacity, but its n type mixes often unstable, expansion of self and contraction can cause its degraded in the charge and discharge process, stability problem in long-term circulation is difficult to solve, and application is restricted.Metal oxide has accurate faraday's electric capacity characteristic because of it, and specific capacitance is high and receive much concern.Wherein, the RuO that makes of sol-gel process
2Specific capacity up to 768F/g, but RuO
2Cost an arm and a leg, this makes to its research and uses and all is restricted.
Manganese oxide (MnO
2) have and RuO
2Similar character, and manganese oxide (MnO
2) also have aboundresources, low price and an advantage such as environmentally friendly.Manganese wherein can have+1 ,+2 ,+3 ,+4 ,+6 ,+multiple oxidation valence states such as 7, crystal structure is also according to [MnO
6] difference of construction unit arranges, and one dimension tunnel, two-dimensional layer and multiple pore passage structure such as three-dimensional netted are arranged, be the electrode material for super capacitor that has potentiality.
But, because MnO
2Itself be semiconductor, as electrode material, a little less than the ability of its electrical conductivity, the performance of performance is subjected to bigger restriction always.As Wang[X.Y.Wang et.al, J.Power Source140 (2005) 211-215.] and Yue[G.H.Yue et.al, J.Crystal Growth 294 (2006) 385-388.] synthesized the MnO of high-sequential respectively with collosol and gel masterplate method and solvent-thermal method
2Nano-wire array and monocrystalline MnO
2Nano wire, its electrochemical capacitance performance is with respect to common MnO
2Electrode material improves also little, does not surpass 200F/g than electric capacity.
Mix as influence material structure, mould a kind of important technical that improves material property thereby carry out material structure, significant to the modification of chemical power source electrode material, be the extremely promising good solution and the approach of raising material property.Recently, people such as Machefaux [E.Machefauxet.al, J.Powersourcs 165 (2007) 651-655.'s] studies show that MnO
2Carry out γ-Mn of obtaining behind the element doping
1-yA
yO
2-δ(A=Co, Al) the electrode material chemical property significantly improves.As seen, to MnO
2Carrying out element doping is an important channel of improving its ultracapacitor chemical property.Yet Machefaux adopts, and to be electrochemistry prepare this element doping MnO with the method for hydro-thermal reaction combination
2Electrode material, the method very complicated, controlled condition requires high, is unfavorable for large-scale production.
Problem at the existence of Machefaux method, Chinese patent application CN101409152A discloses the preparation method who has proposed a kind of element-doping manganese bioxide electrode material for super capacitor on April 15th, 2009, that is: adopt high-energy ball milling method with among Al, Ti, Ni, the Fe any one, according to putting into the high-energy ball milling jar after the atomic ratio mixing in 0.05: 0.95 with manganese in the manganese dioxide, the agate ball of selecting for use diameter not wait is made ball-milling medium, and ratio of grinding media to material is 20: 1; Add anticaking agent ethanol, with 250 rev/mins ball milling speed, ball milling 15 hours; Treating ball grinder is cooled to after the room temperature, product taken out that 80 ℃ of freeze-day with constant temperature are 48 hours in drying box; Again dried powder is ground with agate mortar, can obtain element substitute doping manganese oxide electrode material for super capacitor.Though this invention cost is low, preparation technology is simple, but the method with ball milling is mixed, uniformity is difficult to accurate control, and the pollution of ball-milling medium etc. is difficult to effectively avoid in the mechanical milling process, though the industrialization of method is feasible, but will reach the degree of element doping by ball milling, the efficient of this method also is worth discussion.The present invention comes therefrom.
Summary of the invention
The object of the invention is to provide a kind of element-doping manganese bioxide electrode material for super capacitor preparation method, solved prior art use material with carbon element do electrode material for super capacitor littler than electric capacity, cost an arm and a leg as electrode material for super capacitor and poisonous and adopt MnO merely with metal oxide containing precious metals
2A little less than the electronic conduction ability, and the existing method very complicated that manganese dioxide is carried out the element doping modification, the demanding shortcoming of controlled condition.
In order to solve these problems of the prior art, technical scheme provided by the invention is:
A kind of preparation method of element-doping manganese bioxide electrode material for super capacitor is characterized in that said method comprising the steps of:
(1) with the synthetic LiA of suitable method with spinel structure
xMn
2-xO
4Powder body material; Wherein A is selected from Ti, Ni, Sn, Co, Zn, Al metal interpolation element, and x is in 0.01～0.25 scope
(2) LiA that (1) step is obtained
xMn
2-xO
4Powder body material uses lithium ion to deviate from agent under the condition of not destroying presoma spinelle configuration to take off lithium and obtain ultracapacitor with element substitute doping MnO
2Electrode material.
Preferably, the synthetic LiA of described step (1) with spinel structure
xMn
2-xO
4The method of powder body material is selected from solid phase molten-salt reaction method, sol-gal process, coprecipitation; Wherein A is selected from Ti, Ni, Sn, Co, Zn, Al metal interpolation element, and x is in 0.01～0.25 scope.
Preferably, the LiA of described solid phase molten-salt reaction method synthetic spinel structure
xMn
2-xO
4Powder body material comprises with manganese source material, lithium source material and adds the mixed back of element material and calcined 24-48 hour down at temperature 850-970 ℃ that cooling makes the LiA with spinel structure
xMn
2-xO
4Powder body material; Wherein A is selected from Ti, Ni, Sn, Co, Zn, Al metal interpolation element, and x is in 0.01～0.25 scope.
Preferably, manganese source material powder mixes in A/Mn mol ratio 0.2-0.25 ratio with the interpolation element material in the described method; Wherein A is selected from Ti, Ni, Sn, Co, Zn, Al metal interpolation element.
Preferably, lithium ion is deviate from agent and is selected from hydrochloric acid, nitric acid and sulfuric acid in the described method.
Preferably, when adopting sulfuric acid to take off the lithium reaction, the described lithium method of taking off comprises the spinel structure LiA that will obtain
xMn
2-xO
4Powder is suspended in the pure water, under stirring condition, add sulfuric acid solution and keep temperature not to be higher than 50 ℃, pH reaches 0.5-2 until slurry, continue to stir 1 hour, with reacted dope filtration, be washed to eluate and be neutral, vacuumize obtains element substitute doping MnO under 90 ℃ the temperature conditions not being higher than to leach thing
2Electrode material; Wherein A is selected from Ti, Ni, Sn, Co, Zn, Al metal interpolation element, and x is in 0.01～0.25 scope.
Adopt in the technical scheme of the present invention and be applied to the synthetic presoma spinel-type LiA of anode material for lithium-ion batteries production method with appropriate powder characteristics
xMn
2-xO
4Powder, the even doping of element of manganese dioxide and the spinel structure of manganese dioxide are moulded on the realization lattice structure aspect, and then powder immersion, washing, filtration, the drying process used always in the employing chemical process, the precursor powder material that washing by soaking makes under the condition of controlling acidity and temperature removes lithium, and filtration drying, make the MnO that element evenly mixes
2Powder.
When adopting the solid phase molten-salt reaction method, technical scheme of the present invention by with manganese source material, lithium source material and with add element material and carry out granulation after mixed, temperature programmed control calcining then comprises that low temperature presintering and high-temperature calcination form the LiA with spinel structure
xMn
2-xO
4Powder body material; The LiA that will have spinel structure
xMn
2-xO
4Take off lithium after powder body material is pulverized, wash the dry required element doping MnO2 powder that obtains.
Its concrete technological process can adopt following steps to carry out:
A: spinelle LiA
xMn
2-xO
4Synthesizing of powder body material
The electrolytic manganese dioxide powder is manufactured the powder of about 20 microns of particle diameters, again with add element material, as Ni (OH)
2Press A/Mn mol ratio 0.2-0.25, the ratio of Li/Mn mol ratio 0.5 is mixed in the agitation grinding mill fully, with the temperature programmed control Muffle furnace mixture is calcined 24-48 hour down at 850-970 ℃, and cooling makes the LiA with spinel structure
xMn
2-xO
4Powder body material.
B, element substitute doping MnO
2Preparation
With the spinelle LiA that makes
xMn
2-xO
4Powder is suspended in the pure water, under stirring condition, add sulfuric acid solution and keep temperature not to be higher than 50 ℃, pH reaches 0.5-2 until slurry, continue to stir 1 hour, and with reacted slurries suction filtration or use the filter press press filtration, removed moisture and be washed to eluate repeatedly and be neutrality, leach thing not being higher than vacuumize under 90 ℃ the temperature conditions, promptly obtain element doping MnO2 powder.
The MnO of the inventive method preparation
2Powder, the Mn in the lattice partly are doped element and replace, and the doped chemical replacement evenly, and the industrialization maturity height of method is a preparation approach that has the ultracapacitor of potentiality with the manganese oxide electrode material.
With respect to scheme of the prior art, advantage of the present invention is:
Compared with prior art, the present invention is by synthetic precursor powder material---and the element with spinel structure replaces LiMn2O4, realizes the even substitute doping of doped chemical, has avoided existing doping techniques to mix and has controlled the problem of difficulty; The technology of the synthetic precursor powder material of the present invention is comparatively ripe in addition, and some technology has been successfully applied to suitability for industrialized production, and mature technical route is reliable, more is applicable to industrialization.
Description of drawings
Below in conjunction with drawings and Examples the present invention is further described:
Fig. 1 is preparation technology's flow chart of element-doping manganese bioxide electrode material for super capacitor of the present invention;
Fig. 2 is the cyclic voltammetry scan curve of the element-doping manganese bioxide electrode material of the embodiment of the invention 1 preparation.
Fig. 3 is the constant current charge-discharge curve of the substitute doping manganese oxide electrode material of the embodiment of the invention 2 preparations.
Embodiment
Below in conjunction with specific embodiment such scheme is described further.Should be understood that these embodiment are used to the present invention is described and are not limited to limit the scope of the invention.The implementation condition that adopts among the embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in the normal experiment.
The preparation of embodiment 1:Ni element-doping manganese bioxide electrode material
Electrolytic manganese dioxide powder and Ni (OH) with about 20 microns of particle diameters
2Press Ni/Mn mol ratio 0.2, the ratio agitation grinding of Li/Mn mol ratio 0.5 mixes fully, with the temperature programmed control Muffle furnace mixture is calcined 48 hours down at 850-970 ℃, and cooling makes the LiNi with spinel structure
xMn
2-xO
4Powder body material.With the spinelle LiNi that makes
xMn
2-xO
4Powder is suspended in the pure water, under stirring condition, slowly add sulfuric acid solution, the control temperature is not higher than 50 ℃, and pH reaches 0.5-2 until slurry, continue to stir 1 hour, reacted slurries centrifugation, the supernatant liquor that inclines, suction filtration also are washed to eluate repeatedly and are neutral, leach thing and be not higher than vacuumize under 90 ℃ the temperature conditions, obtain nickel doped with Mn O2 powder.
With the Ni doping manganese bioxide electrode material for preparing is positive pole, and graphite electrode is a negative pole, and the Ag/AgCl electrode is a reference electrode, and 1MNa2SO4 is an electrolyte, forms three electrode test systems the chemical property of material is tested.Cyclic voltammetry scan speed 10mv/s, sweep interval 0.0-1.0V; Constant current charge-discharge electric current 200ma/g, voltage range 0-1.0v.Ni dopping manganese dioxide electrode is back than electric capacity 168f/g 500 circulations.
The preparation of embodiment 2Ti element-doping manganese bioxide electrode material
It is described to press embodiment 1, prepares titanium doped manganese oxide electrode material with the following anatase titanium dioxide TiO2 of 1250 orders powder;
With the Ti doping manganese bioxide electrode material for preparing is positive pole, and graphite electrode is a negative pole, and the Ag/AgCl electrode is a reference electrode, and 1MNa2SO4 is an electrolyte, forms three electrode test systems the chemical property of material is tested.Cyclic voltammetry scan speed 10mv/s, sweep interval 0.0-1.0V; Constant current charge-discharge electric current 200mA/g, voltage range 0-1.0v.Ti dopping manganese dioxide electrode is back than electric capacity 163f/g 500 circulations.
The preparation of embodiment 3Co element-doping manganese bioxide electrode material
It is described to press embodiment 1, prepares cobalt doping manganese oxide electrode material with the following Co2O3 powder of 1250 orders;
With the Co doping manganese bioxide electrode material for preparing is positive pole, and graphite electrode is a negative pole, and the Ag/AgCl electrode is a reference electrode, and 1MNa2SO4 is an electrolyte, forms three electrode test systems the chemical property of material is tested.Cyclic voltammetry scan speed 10mv/s, sweep interval 0.0-1.0V; Constant current charge-discharge electric current 200mA/g, voltage range 0-1.0v.Co dopping manganese dioxide electrode is back than electric capacity 178f/g 500 circulations.
Above-mentioned example only is explanation technical conceive of the present invention and characteristics, and its purpose is to allow the people who is familiar with this technology can understand content of the present invention and enforcement according to this, can not limit protection scope of the present invention with this.All equivalent transformations that spirit is done according to the present invention or modification all should be encompassed within protection scope of the present invention.
Claims (3)
1. the preparation method of an element-doping manganese bioxide electrode material for super capacitor is characterized in that said method comprising the steps of:
(1) with solid phase molten-salt reaction method, sol-gal process, the synthetic LiA of coprecipitation with spinel structure
xMn
2-xO
4Powder body material; Wherein A is selected from Ti, Ni, Sn, Co, Zn, Al metal interpolation element, and x is in 0.01～0.25 scope;
(2) LiA that (1) step is obtained
xMn
2-xO
4Powder body material uses lithium ion to deviate from agent under the condition of not destroying presoma spinelle configuration to take off lithium and obtain ultracapacitor with element substitute doping MnO
2Electrode material; Described lithium ion is deviate from agent and is selected from hydrochloric acid, nitric acid and sulfuric acid;
Wherein when adopting sulfuric acid to take off the lithium reaction, the described lithium method of taking off comprises the spinel structure LiA that will obtain
xMn
2-xO
4Powder is suspended in the pure water, under stirring condition, add sulfuric acid solution and keep temperature not to be higher than 50 ℃, pH reaches 0.5-2 until slurry, continue to stir 1 hour, with reacted dope filtration, be washed to eluate and be neutral, vacuumize obtains element substitute doping MnO under 90 ℃ the temperature conditions not being higher than to leach thing
2Electrode material.
2. method according to claim 1 is characterized in that the LiA of described solid phase molten-salt reaction method synthetic spinel structure
xMn
2-xO
4Powder body material comprises with manganese source material, lithium source material and adds the mixed back of element material and calcined 24-48 hour down at temperature 850-970 ℃ that cooling makes the LiA with spinel structure
xMn
2-xO
4Powder body material; Wherein A is selected from Ti, Ni, Sn, Co, Zn, Al metal interpolation element, and x is in 0.01～0.25 scope.
3. method according to claim 2 is characterized in that manganese source material in the described method is that the ratio of 0.2-0.25 is mixed with adding element material in the A/Mn mol ratio; Wherein A is selected from Ti, Ni, Sn, Co, Zn, Al metal interpolation element.
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| CN101950681B (en) * | 2010-09-09 | 2012-07-04 | 江西财经大学 | Method for preparing manganese oxide electrode material for super capacitor by solvothermal method |
| CN103117384B (en) * | 2012-11-09 | 2015-11-25 | 湘潭大学 | A kind of anion X doping λ-MnO 2lithium primary battery positive electrode and preparation method |
| CN103811190B (en) * | 2014-01-16 | 2016-04-13 | 天津大学 | The coated porous manganese dioxide composite electrode material of stibium doping stannic oxide and preparation |
| CN104355334B (en) * | 2014-10-22 | 2016-08-31 | 太原理工大学 | There is superelevation birnessite type manganese oxide powder body than capacitance characteristic and preparation method and application |
| CN104556234B (en) * | 2014-10-24 | 2016-02-03 | 信阳师范学院 | A kind of mesoporous carbon hydridization nano material of manganese dioxide and preparation method thereof |
| CN105244181B (en) * | 2015-08-24 | 2019-01-08 | 太原理工大学 | Spinel-type metal oxide of high specific capacitance characteristic and the preparation method and application thereof |
| CN106910642B (en) * | 2015-12-22 | 2019-06-07 | 比亚迪股份有限公司 | A kind of supercapacitor and preparation method thereof |
| CN111689523B (en) * | 2019-03-11 | 2022-03-15 | 南京理工大学 | Metallic chromium doped delta-MnO2Preparation method of nanosheet |
| CN112723416A (en) * | 2021-01-05 | 2021-04-30 | 贵州大学 | Method for efficiently preparing potassium and sodium co-doped sheet layered manganese dioxide |
| CN115849453B (en) * | 2022-12-16 | 2024-05-03 | 惠州亿纬锂能股份有限公司 | Ternary co-doped manganese dioxide material and preparation method and application thereof |
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Owner name: SUZHOU JUXINYUAN INVESTMENT MANAGEMENT CO., LTD. Free format text: FORMER OWNER: SUZHOU YOUR BEST NEW MATERIALS CO., LTD. Effective date: 20150422 |
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Effective date of registration: 20160504 Address after: 215100, Jiangsu, Wuzhong District province Suzhou Yue Street North Guandu Road No. 2, 38, east 4 Patentee after: SUZHOU XINYIBO ELECTRONIC TECHNOLOGY CO., LTD. Address before: 215124, No. 22 Xiang Xiang Road, Yue Xi Street, Wuzhong District, Jiangsu, Suzhou Patentee before: Suzhou poly source Cci Capital Ltd |
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Effective date of registration: 20191118 Address after: 215000 No.22, Youxiang Road, Yuexi street, Wuzhong Economic Development Zone, Suzhou City, Jiangsu Province Patentee after: SUZHOU YOURBEST NEW-TYPE MATERIALS CO., LTD. Address before: 215100, Jiangsu, Wuzhong District province Suzhou Yue Street North Guandu Road No. 2, 38, east 4 Patentee before: SUZHOU XINYIBO ELECTRONIC TECHNOLOGY CO., LTD. |
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