CN106449167B - A kind of simple and quick raising MnO2The method of based super capacitor specific capacity - Google Patents
A kind of simple and quick raising MnO2The method of based super capacitor specific capacity Download PDFInfo
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Abstract
The invention discloses a kind of simple and quick raising MnO2The method of based super capacitor specific capacity.This method comprises the following steps: (1) by MnO2Base electrode is immersed in MnSO4In solution, make Mn2+It is adsorbed on MnO2In tunnel；(2) by the MnO after immersion2Base electrode is for making MnO2Based super capacitor increases proton and participates in energy storage degree, improves MnO2The specific capacity of based super capacitor.Operation of the present invention is simple, low in cost, and effect is obvious, can effectively improve MnO2Tunnel structure, improve MnO2The specific capacity of base electrode supercapacitor increases MnO2The utilization efficiency of base electrode material.The method of the present invention can be applied in the production process of manganese base fake capacitance electrode, and novel electrolyte with manganese ions can also be produced as principle.
Description
Technical field
The invention belongs to electric chemical super capacitor fields, and in particular to a kind of simple and quick raising manganese dioxide base is super
The method of capacitor specific discharge capacity.
Background technique
Currently, MnO2The advantages that based super capacitor is low in cost with its, environmentally friendly, highly-safe causes to study people
Member note that however MnO2Based super capacitor also faces problems, if actual specific capacity is not high, cycle life and stability
It is undesirable etc..Mn oxide has biggish tunnel structure, is suitable for the insertion abjection of electrolyte cation and proton, from there through
Reversible faraday's reaction realizes energy storage.But electrolyte cation is larger there are radius thus migration velocity is relatively slow, Transfer Depth
It is shallower and further result in the not high problem of actual specific capacity；And proton participates in energy storage and is easy to produce interphase MnOOH and occurs
Disproportionated reaction thereby results in the reduction of active material so that reduced performance.Thus how to regulate and control MnO2Energy storage behavior, by
The process of this regulation electrolyte ion and proton insertion abjection becomes balance specific capacity and cycle life, optimization Mn oxide electricity
The key of polarity energy.
Summary of the invention
In order to improve MnO2The specific capacity of based super capacitor, we make Mn by the method impregnated2+It is adsorbed on MnO2Tunnel
In road.Due in aqueous electrolyte, Mn2+It is easily absorbing in α-MnO22 × 2 tunnels and δ-MnO2Interlayer tunnel,
Mn is made using the method for immersion2+It is formed into above-mentioned tunnel similar to Mn3O4Structure, and thus regulate and control MnO2Tunnel
Structure improves practical MnO to reach so that proton, which more easily enters, participates in energy storage in tunnel2Based super capacitor specific volume
The purpose of amount.
The present invention is achieved through the following technical solutions.
A kind of simple and quick raising MnO2The method of based super capacitor specific capacity, includes the following steps:
(1) by MnO2Base electrode is immersed in MnSO4In solution, make Mn2+It is adsorbed on MnO2In tunnel；
(2) by the MnO after immersion2Base electrode is for making MnO2Based super capacitor, due to Mn2+It is adsorbed on MnO2Tunnel
It is middle to form similar Mn3O4Structure, change MnO2Tunnel structure, to make MnO2Based super capacitor matter in thermal energy storage process
Son more easily enters and participates in energy storage in tunnel, and then improves MnO2The specific capacity of based super capacitor.
Further, in step (1), the time of the immersion is 2 ~ 30 min.
Further, in step (1), the MnSO4The concentration of solution is 0.1 ~ 0.5 M.
Further, in step (1), the MnO2Base electrode includes α-MnO2Base electrode or δ-MnO2Base electrode.
Further, the α-MnO2Base electrode is prepared by hydro-thermal method, is specifically comprised the following steps:
(1) manganese sulfate solution and potassium permanganate solution are stirred, obtain suspension, is cooled to after sealing reaction
Room temperature filters, and washs, dry, obtains α-MnO2Powder；
(2) by α-MnO2Solvent dissolution is added after powder, acetylene black and polytetrafluoroethylene (PTFE) mixing, slurry is made in ultrasonic disperse
Material, slurry obtained are coated in glassy carbon electrode surface, and drying obtains α-MnO2Base electrode.
Further optimize, in step (1), the concentration of the manganese sulfate solution is 0.1-0.5 M, the permanganic acid
The concentration of aqueous solutions of potassium is 0.1 ~ 0.5 M, and the mixed volume ratio of manganese sulfate solution and potassium permanganate solution is 1:1.
Further optimize, in step (1), the time being stirred is 20 ~ 50 min.
Further optimize, in step (1), the temperature of the reaction is 120 ~ 180 DEG C, and the time is 18 ~ 32h.
Further optimize, in step (2), α-MnO2The mass ratio of powder, acetylene black and polytetrafluoroethylene (PTFE) is 8 ~ 6:1
~3:1。
Further optimize, in step (2), the solvent includes ethyl alcohol.
Further optimize, in step (2), the time of the ultrasound is 20 ~ 60 min.
Further optimize, in step (2), the amount of the coating is 1 ~ 8 g/m2。
Further, the δ-MnO2Base electrode is obtained by electrodeposition process, is specifically comprised the following steps:
(1) carbon paper is successively used to dehydrated alcohol, hydrochloric acid and acetone ultrasonic treatment；
(2) using treated carbon paper as working electrode, using Amperometric i-t curve method, three electrode electricity are heavy
Product obtains δ-MnO2Base electrode is dried for standby.
Further optimize, in step (1), the concentration of the hydrochloric acid is 0.1 ~ 0.5 M.
Further optimize, in step (1), the time of the ultrasonic treatment is 10 ~ 30 min.
Further optimize, in step (2), three electrodes are using treated carbon paper as working electrode, and platinum guaze is to electricity
Pole, saturated calomel electrode are reference electrode.
Further optimize, in step (2), the electrolyte that electrodeposition process uses is molten for acetic acid manganese solution and sodium sulphate
The mixed solution of liquid, the concentration of the acetic acid manganese solution are 0.1 ~ 0.5 M, and the concentration of the metabisulfite solution is 0.1 ~ 0.5 M,
The mixed volume ratio of acetic acid manganese solution and metabisulfite solution is 1:1 ~ 3.
Further optimize, in step (2), electrodeposition process are as follows: first in 0.4 V electro-deposition, 40 s, then exist
0.45 V electro-deposition, 300 ~ 600 s.
To MnO before and after impregnating2The performance of base electrode, including chemical property, microscopic appearance feature and Raman spectrum carry out
Comparative analysis.
The method of the present invention can be applied in the production process of manganese base fake capacitance electrode, can also produce as principle novel
Electrolyte with manganese ions.
Compared with prior art, the invention has the advantages that and the utility model has the advantages that
(1) the method for the present invention is easy to operate, low in cost, and effect is obvious；
(2) present invention passes through regulation MnO2Tunnel structure, thus increase proton participate in energy storage degree, improve MnO2
The specific capacity of based super capacitor, improves MnO2Based super capacitor is MnO in the performance of charge and discharge process2Base super capacitor
Solid technical foundation is laid in the further development of device.
Detailed description of the invention
Fig. 1 is α-MnO2With δ-MnO2X-ray diffraction (XRD) figure spectrum；
Fig. 2 is α-MnO in embodiment 12SEM (SEM) image；
Fig. 3 is that front and back α-MnO is impregnated in embodiment 12The electrochemical property test figure of base electrode；
Fig. 4 a is δ-MnO before impregnating in embodiment 22SEM (SEM) image；
Fig. 4 b is δ-MnO after impregnating in embodiment 22SEM (SEM) image；
Fig. 5 is that front and back δ-MnO is impregnated in embodiment 22The electrochemical property test figure of base electrode；
Fig. 6 is δ-MnO in embodiment 22Raman spectrum of the base electrode under open-circuit condition before and after immersion.
Specific embodiment
The present invention is further elaborated with reference to embodiments, but the present invention is not limited to following embodiments.
Embodiment 1
α-MnO2Base electrode:
(1) hydro-thermal method prepares α-MnO2Powder: MnSO is weighed41.352 g of quality is dissolved in 60 mL water, weighs KMnO4
1.264 g of quality is dissolved in 60mL water, then mixes above two solution with volume ratio 1:1, and stirring continues 20 min, obtains
It to suspension, is transferred in reaction kettle, seals, 160 DEG C of 24 h of reaction, water drenching is cooled to room temperature, and is filtered, washing, 80 DEG C of dryings 8
H obtains α-MnO2Powder；
Obtained α-MnO2The XRD diagram of powder is as shown in Figure 1, as shown in Figure 1, the α-MnO as made from hydro-thermal method2Powder
With the α-MnO of standard PDF card2Unanimously；
Obtained α-MnO2The SEM of powder schemes as shown in Fig. 2, as shown in Figure 2, obtained α-MnO2Powder is nano whiskers.
(2) it prepares slurry: weighing α-MnO2Powder (8 mg), acetylene black (1 mg) and PTFE(1 mg), add ethyl alcohol to mix
Dissolution, 20 min of ultrasonic disperse obtain slurry；
(3) it determines quality: cutting one block of copper foil as carrier, coating slurry 7g/m2, active matter in electrode is calculated with difference assay
0.1 mg of amount of matter, obtains α-MnO2Base electrode；
(4) to obtained α-MnO2Base electrode carries out cyclic voltammetry measurement；
(5) α-MnO that will be obtained2Base electrode is immersed in the MnSO of 0.5M42min in solution, then will be extra with filter paper
Solution blots, and carries out cyclic voltammetry measurement.
α-MnO2It is α that the sample that base electrode immerses front and back is numbered respectively1、α2, to sample α2It is followed after carrying out 10000 circulations
The test of ring voltammetry.
The cyclic voltammetry curve that cyclic voltammetry measurement obtains is as shown in figure 3, impregnating Mn2+α-MnO afterwards2The ratio of base electrode
Capacitance variations very little；Meanwhile to the α-MnO after infiltration2Base electrode carries out the cyclic voltammetry test result after 10000 circulations
Display specific capacitance is significantly increased.
Embodiment 2
α-MnO2Base electrode:
(1) hydro-thermal method prepares α-MnO2Powder: MnSO is weighed4Quality 1.352g is dissolved in 40 mL water, weighs KMnO4Matter
Amount 1.264g is dissolved in 40 mL water, then mixes above two solution with volume ratio 1:1, and stirring continues 40 min, obtains
Suspension is transferred in reaction kettle, and sealing, 180 DEG C of 18 h of reaction, water drenching is cooled to room temperature, and is filtered, washing, 80 DEG C of dryings 8
H obtains α-MnO2Powder；
Obtained α-MnO2XRD diagram and the SEM figure of powder are similar to Example 1；
(2) it prepares slurry: weighing α-MnO2Powder (6 mg), acetylene black (3 mg) and PTFE(1 mg), add ethyl alcohol to mix
Dissolution, 30 min of ultrasonic disperse obtain slurry；
(3) it determines quality: cutting one block of copper foil as carrier, 2 g/m of coating slurry2, activity in electrode is calculated with difference assay
0.2 mg of amount of substance, obtains α-MnO2Base electrode；
(4) to obtained α-MnO2Base electrode carries out cyclic voltammetry measurement；
(5) α-MnO that will be obtained2Base electrode is immersed in the MnSO of 0.1M430min in solution, then will be extra with filter paper
Solution blots, and carries out cyclic voltammetry measurement.
α-MnO2It is α that the sample that base electrode immerses front and back is numbered respectively3、α4, to sample α4It is followed after carrying out 10000 circulations
The test of ring voltammetry.
The cyclic voltammetry curve that cyclic voltammetry measurement obtains, specific capacity variation is little after immersion, after circulation 10000 times
It is significantly increased.
Embodiment 3
α-MnO2Base electrode:
(1) hydro-thermal method prepares α-MnO2Powder: MnSO is weighed4Quality 1.352g is dissolved in 20 mL water, weighs KMnO4Matter
Amount 1.264g is dissolved in 20 mL water, then mixes above two solution with volume ratio 1:1, and stirring continues 50 min, obtains
Suspension is transferred in reaction kettle, and sealing, 120 DEG C of 32 h of reaction, water drenching is cooled to room temperature, and is filtered, washing, 80 DEG C of dryings 8
H obtains α-MnO2Powder；
Obtained α-MnO2XRD diagram and the SEM figure of powder are similar to Example 1；
(2) it prepares slurry: weighing α-MnO2Powder (7 mg), acetylene black (2 mg) and PTFE(1 mg), add ethyl alcohol to mix
Dissolution, 60 min of ultrasonic disperse obtain slurry；
(3) it determines quality: cutting one block of copper foil as carrier, coating slurry 5g/m2, active matter in electrode is calculated with difference assay
The amount 0.14mg of matter, obtains α-MnO2Base electrode；
(4) to obtained α-MnO2Base electrode carries out cyclic voltammetry measurement；
(5) α-MnO that will be obtained2Base electrode is immersed in the MnSO of 0.2M420min in solution, then will be extra with filter paper
Solution blots, and carries out cyclic voltammetry measurement.
α-MnO2It is α that the sample that base electrode immerses front and back is numbered respectively5、α6, to sample α6It is followed after carrying out 10000 circulations
The test of ring voltammetry.
The cyclic voltammetry curve that cyclic voltammetry measurement obtains, specific capacity variation is little after immersion, after circulation 10000 times
It is significantly increased.
Embodiment 4
δ-MnO2Base electrode:
(1) processing of carbon paper: successively 10 min of ultrasound in dehydrated alcohol, 0.1 M hydrochloric acid and acetone by carbon paper；
(2) using treated carbon paper as working electrode, platinum guaze is to electrode, and saturated calomel electrode (SCE) is reference electrode,
With 0.1M manganese acetate (MnAC2) solution and 0.1M sodium sulphate (Na2SO4) solution mixed solution be electrolyte, acetic acid manganese solution
Mixed volume ratio with metabisulfite solution is 1:1, first deposits 40 in 0.4 V using Amperometric i-t curve method
S, then 600 s are deposited in 0.45 V, the quality that active material is calculated by the quantity of electric charge is 0.102 mg, and 140 DEG C of 30 min of baking are obtained
To δ-MnO2Base electrode；
Obtained δ-MnO2The XRD spectrum of base electrode is as shown in fig. 1, as shown in Figure 1, obtained δ-MnO2Base electrode with
δ-the MnO of standard PDF card2Unanimously, it is possible to determine that be pure phase；
(3) δ-MnO that will be obtained2Base electrode carries out cyclic voltammetry measurement；
(4) by δ-MnO2Base electrode is immersed in 0.2M MnSO430min in solution takes out, is dried for standby.
δ-MnO2It is δ that the sample that base electrode immerses front and back is numbered respectively1、δ2, and to the δ-MnO for impregnating front and back2Base electrode into
10000 loop tests of row.
Fig. 4 a is the δ-MnO before impregnating2Base electrode SEM figure looks, Fig. 4 b are the δ-MnO after impregnating2Base electrode SEM figure
Looks；By Fig. 4 a and Fig. 4 b it is found that δ-MnO2Base electrode impregnates Mn2+Front and back pattern is without significant change.
Impregnate the δ-MnO of front and back210000 circulation results of base electrode are as shown in figure 5, as shown in Figure 5, impregnate Mn2+Afterwards
δ-MnO2Base electrode specific capacitance can undergo one first to increase to reduce afterwards, finally gradually stable process, the specific capacity ratio after stablizing
δ-MnO without immersion2Base electrode specific capacity height nearly 70%.
Impregnate the δ-MnO of front and back2The Raman map of base electrode is as shown in Figure 6, wherein (a) is the δ-MnO before impregnating2Base electricity
The Raman map of pole, the δ-MnO after (b) impregnating2Raman map of the base electrode into the circulation of 1 CV excessively；Intended by (a) and (b) in Fig. 6
Analysis is closed it is found that δ-MnO2Base electrode is impregnating Mn2+After there are 656 cm-1New peak, this is counted as Mn3O4Feature
Peak.It can be seen that Mn2+MnO is entered2Lattice structure in, and part forms similar Mn3O4Structure, to change
MnO2Tunnel structure, increase ion participate in energy storage degree, substantially increase the chemical property of material.
Embodiment 5
δ-MnO2Base electrode:
(1) processing of carbon paper: successively 30 min of ultrasound in dehydrated alcohol, 0.5 M hydrochloric acid and acetone by carbon paper；
(2) using treated carbon paper as working electrode, platinum guaze is to electrode, and saturated calomel electrode (SCE) is reference electrode,
With 0.2M manganese acetate (MnAC2) solution and 0.2M sodium sulphate (Na2SO4) solution mixed solution be electrolyte, acetic acid manganese solution
Mixed volume ratio with metabisulfite solution is 1:3, first deposits 40 in 0.4 V using Amperometric i-t curve method
S, then 300 s are deposited in 0.45 V, the quality that active material is calculated by the quantity of electric charge is 0.051 mg, and 140 DEG C of 30 min of baking are obtained
To δ-MnO2Base electrode；
(3) δ-MnO that will be obtained2Base electrode carries out cyclic voltammetry measurement；
(4) by δ-MnO2Base electrode is immersed in 0.5M MnSO42 min in solution takes out, is dried for standby.
To the δ-MnO for impregnating front and back2Base electrode carries out 10000 loop tests.The specific capacity of electrode is very stable before impregnating,
And δ-the MnO after impregnating2Base electrode is recycled through 10000 times, and specific capacitance can first increase to be reduced afterwards, finally gradually stable, after stablizing
Specific capacity than no immersion δ-MnO2Base electrode specific capacity is high by about 70%.
Embodiment 6
δ-MnO2Base electrode:
(1) processing of carbon paper: successively 20 min of ultrasound in dehydrated alcohol, 0.3 M hydrochloric acid and acetone by carbon paper；
(2) using treated carbon paper as working electrode, platinum guaze is to electrode, and saturated calomel electrode (SCE) is reference electrode,
With 0.5M manganese acetate (MnAC2) solution and 0.5M sodium sulphate (Na2SO4) solution mixed solution be electrolyte, acetic acid manganese solution
Mixed volume ratio with metabisulfite solution is 1:2, first deposits 40 in 0.4 V using Amperometric i-t curve method
S, then 400 s are deposited in 0.45 V, the quality that active material is calculated by the quantity of electric charge is 0.08 mg, and 140 DEG C of 30 min of baking are obtained
To δ-MnO2Base electrode；
(3) δ-MnO that will be obtained2Base electrode carries out cyclic voltammetry measurement；
(4) by δ-MnO2Base electrode is immersed in 0.1M MnSO415 min in solution takes out, is dried for standby.
To the δ-MnO for impregnating front and back2Base electrode carries out 10000 loop tests.The specific capacity of electrode is very stable before impregnating,
And δ-the MnO after impregnating2Base electrode is recycled through 10000 times, and specific capacitance can first increase to be reduced afterwards, finally gradually stable, after stablizing
Specific capacity than no immersion δ-MnO2Base electrode specific capacity is high by about 70%.
Claims (4)
1. a kind of simple and quick raising MnO2The method of based super capacitor specific capacity, which comprises the steps of:
(1) by MnO2Base electrode is immersed in MnSO4Solution makes Mn2+It is adsorbed on MnO2In tunnel；The MnO2Base electrode includes α-
MnO2Base electrode or δ-MnO2Base electrode；
α-the MnO2Base electrode is prepared by hydro-thermal method, is specifically comprised the following steps:
(a) manganese sulfate solution and potassium permanganate solution are stirred, obtain suspension, is cooled to room after sealing reaction
Temperature filters, and washs, dry, obtains α-MnO2Powder；The concentration of the manganese sulfate solution is 0.1 ~ 0.5 M, the permanganic acid
The concentration of aqueous solutions of potassium is 0.1 ~ 0.5 M, and the mixed volume ratio of manganese sulfate solution and potassium permanganate solution is 1:1；It is described
The time being stirred is 20 ~ 50 min；The temperature of the reaction is 120 ~ 180 DEG C, and the time is 18 ~ 32 h；The manganese sulfate
The concentration of aqueous solution is 0.1 ~ 0.5 M, and the concentration of the potassium permanganate solution is 0.1 ~ 0.5 M, manganese sulfate solution and height
The mixed volume ratio of mangaic acid aqueous solutions of potassium is 1:1；The time being stirred is 20 ~ 50 min；The temperature of the reaction is
120 ~ 180 DEG C, the time is 18 ~ 32 h；
(b) by α-MnO2Solvent dissolution is added after powder, acetylene black and polytetrafluoroethylene (PTFE) mixing, slurry is made in ultrasonic disperse, is made
Slurry be coated in glassy carbon electrode surface, drying, obtain α-MnO2Base electrode；
δ-the MnO2Base electrode is obtained by electrodeposition process, is specifically comprised the following steps:
(A) carbon paper is successively used to dehydrated alcohol, hydrochloric acid and acetone ultrasonic treatment；The concentration of the hydrochloric acid is 0.1 ~ 0.5 M；Institute
The time for stating ultrasonic treatment is 10 ~ 30 min；
(B) using treated carbon paper as working electrode, using Amperometric i-t curve method, three electrode electro-deposition are obtained
To δ-MnO2Base electrode is dried for standby；Three electrodes are using treated carbon paper as working electrode, and platinum guaze is to be saturated sweet to electrode
Mercury electrode is reference electrode；The electrolyte that electrodeposition process uses is the mixed solution of acetic acid manganese solution and metabisulfite solution, institute
The concentration for stating acetic acid manganese solution is 0.1 ~ 0.5 M, and the concentration of the metabisulfite solution is 0.1 ~ 0.5 M, acetic acid manganese solution and sulphur
The mixed volume ratio of acid sodium solution is 1:1 ~ 3；
(2) by the MnO after immersion2Base electrode is for making MnO2Based super capacitor, due to Mn2+It is adsorbed on MnO2Shape in tunnel
At similar Mn3O4Structure, change MnO2Tunnel structure, to make MnO2Proton is more in thermal energy storage process for based super capacitor
Add to be easily accessible in tunnel and participate in energy storage, that is, improves MnO2The specific capacity of based super capacitor.
2. a kind of simple and quick raising MnO according to claim 12The method of based super capacitor specific capacity, feature exist
In, in step (b), α-MnO2The mass ratio of powder, acetylene black and polytetrafluoroethylene (PTFE) is 8 ~ 6:1 ~ 3:1；The solvent includes second
Alcohol；The time of the ultrasound is 20 ~ 60 min；The amount of the coating is 1 ~ 8 g/m2。
3. a kind of simple and quick raising MnO according to claim 12The method of based super capacitor specific capacity, feature exist
In, in step (B), electrodeposition process are as follows: first in 0.4 V electro-deposition, 40 s, then in 0.45 V electro-deposition, 300 ~ 600 s.
4. a kind of simple and quick raising MnO according to claim 12The method of based super capacitor specific capacity, feature exist
In in step (1), the time of the immersion is 2 ~ 30 min；The MnSO4The concentration of solution is 0.1 ~ 0.5 M.
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