CN107045948B - NaxMnO2Positive electrode, preparation method and applications - Google Patents
NaxMnO2Positive electrode, preparation method and applications Download PDFInfo
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- CN107045948B CN107045948B CN201710230470.0A CN201710230470A CN107045948B CN 107045948 B CN107045948 B CN 107045948B CN 201710230470 A CN201710230470 A CN 201710230470A CN 107045948 B CN107045948 B CN 107045948B
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- carbon cloth
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- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 38
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 18
- 239000004744 fabric Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910019898 NaxMnO2 Inorganic materials 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 26
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 238000004070 electrodeposition Methods 0.000 claims description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 238000002203 pretreatment Methods 0.000 claims description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract description 14
- 229910021607 Silver chloride Inorganic materials 0.000 abstract description 5
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 abstract description 5
- 239000002105 nanoparticle Substances 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 28
- 239000003990 capacitor Substances 0.000 description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 239000011572 manganese Substances 0.000 description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 229910052938 sodium sulfate Inorganic materials 0.000 description 6
- 238000007599 discharging Methods 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000007832 Na2SO4 Substances 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 238000010306 acid treatment Methods 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229920002301 cellulose acetate Polymers 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000002955 isolation Methods 0.000 description 3
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical class [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 239000002985 plastic film Substances 0.000 description 3
- 229920006255 plastic film Polymers 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 235000011152 sodium sulphate Nutrition 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- -1 (Na+And K+) Chemical class 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000009194 climbing Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 kind of NaxMnO2Positive electrode, preparation method and applications, step are：（1）Pass through the Mn to being grown on carbon cloth3O4Nano-particles self assemble at nm wall array carry out hydro-thermal, to form the Na of high Na contents0.55MnO2The nm wall array that nanometer sheet is self-assembled into.Na0.55MnO2Nm wall array operating potential window can expand to 0~1.3V（vs.Ag/AgCl）, specific capacitance can reach 366Fg‑1；With Na0.55MnO2For positive electrode, carbon-coated Fe is utilized3O4Nanometer stick array is prepared for the Na of 2.6V ultra-wide operating potential windows as cathode0.55MnO2//Fe3O4@C water system Asymmetric Supercapacitors.The ultracapacitor not only has the general character of ultracapacitor：High power density, overlength cycle life, and the energy density of the operating potential window (2.6V) with ultra-wide, superelevation（87Whkg‑1）.
Description
Technical field
The invention patent relates to the Na of high Na contentsxMnO2Positive electrode, preparation method and this positive electrode structure of utilization
The method for building the water system Asymmetric Supercapacitor of 2.6V ultra-wide potential windows, belongs to electrochemical energy storage technical field.
Background technology
Ultracapacitor is a kind of new and effective secondary power supply between battery and traditional capacitance, has the cycle longevity
Order length, power density height, safety, advantages of environment protection.Its power density ratio battery will be higher by 10 to 100 times, can release moment
Ultrahigh current is put, therefore is highly suitable for electric vehicle.Such as ultracapacitor can be with the high energy electricity such as lithium secondary battery
Pond is used cooperatively as electric vehicle, and super capacitor is used under the operating mode of the high-power output such as startup, climbing, acceleration
Device can greatly improve the performance of electric vehicle.In addition, ultracapacitor is alternatively arranged as stand-by power supply, independent current source
In the fields extensive use such as communication, industry.Therefore, ultracapacitor always is the hot spot of research.
It is further wide seriously to limit ultracapacitor the disadvantage is that energy density is low for aqueous super capacitor most important
General application, so current top priority is exactly to improve the energy density of ultracapacitor.According to density energy formula E=1/
2CV2, energy density (E) is related with its operating potential window (V) and its capacity (C), wherein can be seen that energy is close from formula
There are exponential relationships for degree and operating potential window, therefore raising operating potential window is particularly important.
Due to MnO2With larger specific capacitance and higher oxygen evolution potential (1V), therefore it is super to be very suitable for doing high potential
The electrode material of grade capacitor.But report at present with MnO2For the ultracapacitor such as ACS Nano of base, 6 (5), 4020-
40282012, Advanced Functional Material, 21,2366-2375,2011 equal operating potentials windows 1.6V~
Between 2.0V, energy density is in 20~50Wh kg-1, energy density and potential window are all than relatively limited.Recently, there are several projects
Group includes that this seminar finds to MnO2Carry out pre- embedding cation such as (Na+And K+), it can effectively improve MnO2Electrochemical scholarship and moral conduct
For in MnO2In embedded a large amount of cation it is still extremely difficult.
Invention content
In order to overcome the present situation that current aqueous super capacitor potential window is narrow, energy density is low, the purpose of the present invention is
A kind of Na of high Na contents is providedxMnO2Positive electrode, preparation method and utilization this positive electrode structure 2.6V ultra-wide electricity
The method of the water system Asymmetric Supercapacitor of position window, it has high power characteristic, excellent cycle life, 2.6V simultaneously
The features such as ultra-wide operating potential window, high energy density and low cost and good security performance.
For achieving the above object, the technical solution that the present invention takes is：A kind of NaxMnO2Positive electrode, it is described
NaxMnO2X=0.55 in positive electrode.
Above-mentioned NaxMnO2The preparation process of positive electrode is as follows：
1) it utilizes on the carbon cloth of cathodic electrodeposition method after the pre-treatment and prepares Mn3O4Nm wall array；
2) by Mn3O4Nm wall array is immersed in NaOH solution, then at 120 DEG C~180 DEG C hydro-thermal reaction 12~
25h obtains Na0.55MnO2Nm wall array.
Further, in step 2), the molar concentration of NaOH solution is 0.5~1.5M.
Above-mentioned NaxMnO2Positive electrode builds the application in 2.6V water system Asymmetric Supercapacitors as positive electrode.
Compared with prior art, it is an advantage of the invention that：
(1)Na0.55MnO2Na contents with superelevation, the MnO of high Na contents2With excellent chemical property, including it is super
Wide 0~1.3V of potential window (vs.Ag/AgCl), high specific capacitance 366F g-1And excellent high rate performance and cycle
Stablize.
(2)Na0.55MnO2//Fe3O4@C water system Asymmetric Supercapacitors have ultra-wide operating potential window 2.6V, superelevation
Energy density 87Wh kg-1, wherein the potential window of 2.6V is higher than current all aqueous super capacitors reported.This
Invention is for pushing the further development of aqueous super capacitor to have great importance.
(3) present invention is that electrode material is prepared on carbon cloth, and the use of binder free, conductive agent, preparation flow is short, just
In large-scale production.And the ultracapacitor being assembled into has good flexible folded form, is very suitable for flexible wearable
Electronic equipment.
Description of the drawings
Fig. 1 is the Na in embodiment 10.55MnO2Scanning electron microscope (SEM) photograph.
Fig. 2 is the Na in embodiment 10.55MnO2The charging and discharging curve of electrode material.
Fig. 3 is the Na in embodiment 10.55MnO2//Fe3O4The charging and discharging curve of@C water system Asymmetric Supercapacitors.
Fig. 4 is the Na in embodiment 10.55MnO2//Fe3O4The cycle life figure of@C water system Asymmetric Supercapacitors.
Specific implementation mode
Invention is further described in detail with reference to the accompanying drawings and detailed description：
Embodiment 1
The first step：The pretreatment of carbon cloth：Using 90 DEG C of nitric acid treatment carbon cloth, 6h, surface impurity is removed, is protected in absolute ethyl alcohol
It deposits spare.
Second step：Mn is prepared on carbon cloth using cathodic electrodeposition method3O4Nm wall array.Cathodic electrodeposition method is
Based on three-electrode system, wherein using carbon cloth as working electrode, platinized platinum is to electrode, and Ag/AgCl is reference electrode, and three electrodes are set
Progress -1.8V constant voltages deposit in the sodium sulphate electrolyte by 0.1M manganese acetates and 0.1M, keep 20min, obtain Mn
(OH)2Nm wall array, is then placed in air and ultimately forms Mn3O4Nm wall array.
Third walks：In Mn3O4On the basis of nm wall array, Na is prepared using hydrothermal method0.55MnO2Nm wall array.
It specifically includes：By Mn3O4Nm wall array is immersed in 40mL 1M NaOH solutions, is then transferred into water heating kettle and is carried out hydro-thermal,
Hydrothermal temperature is 160 DEG C, and time 20h finally obtains Na0.55MnO2Nm wall array.Fig. 1 is what the present embodiment obtained
Na0.55MnO2The scanning electron microscope (SEM) photograph of nm wall detects what the present embodiment can obtain being assembled by nanometer sheet completely by test
Na0.55MnO2Nm wall positive electrode.Fig. 2 is Na0.55MnO2The charging and discharging curve of electrode material, detects Na0.55MnO2Material
Potential window can reach 0~1.3V.
4th step：Finally with 1M Na2SO4For electrolyte, Na of the same area is utilized0.55MnO2Anode and Fe3O4@C are negative
Pole is assembled into water system Asymmetric Supercapacitor under the isolation of cellulose acetate membrane diaphragm using metal collector, wherein utilizing aluminium
Plastic film is as encapsulating film.Fig. 3 is Na in the present embodiment0.55MnO2//Fe3O4The charging and discharging curve of@C ultracapacitors, can from figure
To find out that this super capacitor has the steady operation potential window of 2.6V, and there is high coulombic efficiency.Fig. 4 is this implementation
Na in example0.55MnO2//Fe3O4The cycle life figure of@C ultracapacitors, 7000 circles still have 97% capacity retention ratio later,
Show extremely stable electrochemical stability.
Embodiment 2
The first step：The pretreatment of carbon cloth：Using 90 DEG C of nitric acid treatment carbon cloth, 6h, surface impurity is removed, is protected in absolute ethyl alcohol
It deposits spare.
Second step：Mn is prepared on carbon cloth using cathodic electrodeposition method3O4Nm wall array.Cathodic electrodeposition method is
Based on three-electrode system, wherein using carbon cloth as working electrode, platinized platinum is to electrode, and Ag/AgCl is reference electrode, and three electrodes are set
Progress -1.8V constant voltages deposit in the sodium sulphate electrolyte by 0.1M manganese acetates and 0.1M, keep 20min, obtain Mn
(OH)2Nm wall array, is then placed in air and ultimately forms Mn3O4Nm wall array.
Third walks：In Mn3O4On the basis of nm wall array, Na is prepared using hydrothermal method0.55MnO2Nm wall array.
It specifically includes：By Mn3O4Nm wall array is immersed in 40mL 1M NaOH solutions, is then transferred into water heating kettle and is carried out hydro-thermal,
Hydrothermal temperature is 160 DEG C, and time 12h finally obtains Na0.55MnO2Nm wall array.
4th step：Finally with 1M Na2SO4For electrolyte, Na of the same area is utilized0.55MnO2Anode and Fe3O4@C are negative
Pole is assembled into water system Asymmetric Supercapacitor under the isolation of cellulose acetate membrane diaphragm using metal collector, wherein utilizing aluminium
Plastic film is as encapsulating film.
Embodiment 3
The first step：The pretreatment of carbon cloth：Using 90 DEG C of nitric acid treatment carbon cloth, 6h, surface impurity is removed, is protected in absolute ethyl alcohol
It deposits spare.
Second step：Mn is prepared on carbon cloth using cathodic electrodeposition method3O4Nm wall array.Cathodic electrodeposition method is
Based on three-electrode system, wherein using carbon cloth as working electrode, platinized platinum is to electrode, and Ag/AgCl is reference electrode, and three electrodes are set
Progress -1.8V constant voltages deposit in the sodium sulphate electrolyte by 0.1M manganese acetates and 0.1M, keep 20min, obtain Mn
(OH)2Nm wall array, is then placed in air and ultimately forms Mn3O4Nm wall array.
Third walks：In Mn3O4On the basis of nm wall array, Na is prepared using hydrothermal method0.55MnO2Nm wall array.
It specifically includes：By Mn3O4Nm wall array is immersed in 40mL 1M-NaOH solution, is then transferred into water heating kettle and is carried out hydro-thermal,
Hydrothermal temperature is 180 DEG C, and time 12h finally obtains Na0.55MnO2Nm wall array.
4th step：Finally with 1M Na2SO4For electrolyte, Na of the same area is utilized0.55MnO2Anode and Fe3O4@C are negative
Pole is assembled into water system Asymmetric Supercapacitor under the isolation of cellulose acetate membrane diaphragm using metal collector, wherein utilizing aluminium
Plastic film is as encapsulating film.
Claims (5)
1. a kind of NaxMnO2Positive electrode, which is characterized in that the NaxMnO2X=0.55 in positive electrode, by walking as follows
It is rapid to prepare：
1）Using preparing Mn on the carbon cloth of cathodic electrodeposition method after the pre-treatment3O4Nm wall array；
2）By Mn3O4Nm wall array is immersed in NaOH solution, and then 12~25h of hydro-thermal reaction at 120 DEG C~180 DEG C, obtains
To Na0.55MnO2Nm wall array.
2. Na as described in claim 1xMnO2Positive electrode, which is characterized in that step 2）In, the molar concentration of NaOH solution
For 0.5~1.5M.
3. Na as described in claim 1xMnO2The preparation method of positive electrode, which is characterized in that include the following steps：
1）Using preparing Mn on the carbon cloth of cathodic electrodeposition method after the pre-treatment3O4Nm wall array；
2）By Mn3O4Nm wall array is immersed in NaOH solution, and then 12~25h of hydro-thermal reaction at 120 DEG C~180 DEG C, obtains
To Na0.55MnO2Nm wall array.
4. method as claimed in claim 3, which is characterized in that step 2）In, the molar concentration of NaOH solution is 0.5~
1.5M。
5. Na as described in claim 1xMnO2Application of the positive electrode in building 2.6V water system Asymmetric Supercapacitors.
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| CN107946564B (en) * | 2017-11-16 | 2020-05-26 | 武汉理工大学 | Rich in Na4Mn2O5/Na0.7MnO2Composite material and preparation method and application thereof |
| CN108346517B (en) * | 2018-02-06 | 2019-08-20 | 陕西师范大学 | Nanometer Nb2O5The preparation method of/carbon cloth combination electrode material |
| CN109935474A (en) * | 2019-03-16 | 2019-06-25 | 南昌大学 | A kind of magnanimity preparation NaxMnO2The method of electrode material |
| CN111430156B (en) * | 2020-03-20 | 2021-09-07 | 西北工业大学 | Li4Mn5O12Preparation method and use method of nanosheet material |
| CN112374545B (en) * | 2020-11-11 | 2022-03-15 | 湖北大学 | Transition metal ion doped manganous-manganic oxide nanosheet array based on carbon cloth growth and preparation method and application thereof |
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| CN1630126A (en) * | 2004-10-11 | 2005-06-22 | 湘潭大学 | sodium ion battery and method for manufacturing the same |
| KR100982595B1 (en) * | 2005-02-07 | 2010-09-15 | 산요덴키가부시키가이샤 | Positive electrode and nonaqueous electrolyte secondary battery |
| CN102027625B (en) * | 2008-04-07 | 2017-05-03 | 卡内基美浓大学 | Sodium ion based aqueous electrolyte electrochemical secondary energy storage device |
| CN104009252B (en) * | 2013-02-27 | 2017-02-08 | 华为技术有限公司 | Sodium-ion battery and preparation method thereof |
| CN103594707A (en) * | 2013-11-29 | 2014-02-19 | 西南大学 | High-temperature solid-phase synthesis method of one-dimensional nano-sodion cell anode material NaxMnO2 |
| CN105185978A (en) * | 2014-06-20 | 2015-12-23 | 中国科学院物理研究所 | Manganese-containing oxygen compound used as negative active substance, and preparation method and use thereof |
| CN104319424A (en) * | 2014-11-06 | 2015-01-28 | 中国科学技术大学 | Water-system sodium ion battery as well as manufacturing method and application thereof |
| CN104716317B (en) * | 2015-03-09 | 2017-09-12 | 郑州大学 | A kind of sodium-ion battery NaxMnO2The synthetic method of positive electrode |
| CN105489949B (en) * | 2016-01-28 | 2018-06-01 | 吉首大学 | A kind of mixed aqueous solution battery preparation method based on embedding sodium positive electrode |
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Effective date of registration: 20231226 Address after: Room 302, Building 1, No. 297 Zhongshan Gate Street, Xuanwu District, Nanjing City, Jiangsu Province, 210014 Patentee after: Anna (Nanjing) Energy Technology Co.,Ltd. Address before: 210094 No. 200, Xiaolingwei, Jiangsu, Nanjing Patentee before: NANJING University OF SCIENCE AND TECHNOLOGY |