CN106098403B - A kind of ultracapacitor, cathode and preparation method thereof - Google Patents
A kind of ultracapacitor, cathode and preparation method thereof Download PDFInfo
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- 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 ultracapacitors, cathode and preparation method thereof.The cathode includes conductive substrates successively, and it is grown on the amorphous carbon layer on conductive substrates surface, embedded with the manganese oxide particle that grain size is 2nm~40nm in the amorphous carbon layer, the thickness of the amorphous carbon layer is 2nm~300nm, and the manganese oxide particle includes Mn3O4Particle and MnO particles, the Mn3O4The mass ratio of particle and MnO particles is less than 5:8.The present invention is selected by Mn3O4Active material of the manganese and oxygen compound layer of nano particle and MnO nano particles composition as cathode, while utilizing the cyclical stability for the amorphous carbon layer raising cathode for being attached to Mn oxide layer surface；The specific capacity of the cathode prepared improves 50% or more than the prior art, and after cycle charge-discharge 3000 times, specific capacity remains to the original state maintained to close to 100%.
Description
Technical field
The invention belongs to field of new-generation energy storage, more particularly, to a kind of cathode for ultracapacitor and
Preparation method.
Background technology
The energy storage equipment emerging as one, ultracapacitor is as bridging battery and conventional Super capacitor
(SCs) tie has caused the extensive concern of people.Wherein, Asymmetric Supercapacitor (ASCs) is by designing two kinds of electricity
Window different anode in position extends operating voltage window with cathode, to improve its energy density.It is typical asymmetric super
Capacitor is made of faraday's electrode (anode) of cell type as energy source and capacitive electrode (cathode).Carbon-based material
Such as activated carbon (AC), graphene, carbon nanotube etc. is since with excellent electric conductivity, bigger serface and excellent electrochemistry are steady
It is qualitative, it is widely used as the negative material of Asymmetric Supercapacitor.However, carbon-based material low capacity strongly limits
Their applications in high-energy Asymmetric Supercapacitor.
In order to solve this problem, the novel negative material urgent need with high power capacity and high conductivity is probed into.Non- patent
Document (ACS Appl.Mater.Interfaces, 2015,7,11444-11451) discloses a kind of cathode of ultracapacitor
Material grows Mn using manganese acetate and dimethyl sulfoxide (DMSO) as raw material on conductive carbon paper3O4Method and prepare, the negative material
Specific capacity is up to 432mF/cm2；The preparation method has following defect：Preparation process is cumbersome, pollution environment etc., while its specific capacity
Still limited, when for Asymmetric Supercapacitor, significantly limit the specific capacity and energy of Asymmetric Supercapacitor
Density.For example, in hybrid-electric car, all-electric automobile can need in the energy storage device of high power capacity, the super electricity of the prior art
Container is then often difficult to meet demand.
Invention content
For the disadvantages described above or Improvement requirement of the prior art, the present invention provides a kind of cathode for ultracapacitor
And preparation method thereof, its object is to obtain the negative material of height ratio capacity, to increase the application range of ultracapacitor.
To achieve the above object, according to one aspect of the present invention, a kind of cathode, including conductive substrates are provided, and
It is grown on the amorphous carbon layer on conductive substrates surface, the Mn oxide that grain size is 2nm~40nm is embedded in the amorphous carbon layer
Particle, the thickness of the amorphous carbon layer are 2nm~300nm, the manganese oxide particle by 0%~38.5% Mn3O4Particle
And 61.5%~100% MnO particles form.
Preferably, the conductive substrates are carbon cloth, carbon fiber, nickel foam or stainless steel.
Preferably, the Mn3O4The grain size of particle is 3nm~40nm, and the grain size of the MnO particles is 2nm~30nm.
Preferably, the thickness of the amorphous carbon layer is 5nm~50nm.
Preferably, the mass ratio of the manganese oxide particle and the amorphous carbon layer is 0.039:1~118:1.
As it is further preferred that the mass ratio of the manganese oxide particle and the amorphous carbon layer is 6:1~20:1.
Other side according to the invention additionally provides a kind of preparation method of above-mentioned cathode, includes the following steps：
S1. under air-proof condition, conductive substrates are placed in MnO2In precursor solution, 85 DEG C~120 DEG C heating 15min~
360min, acquisition are attached with MnO2Conductive substrates；The MnO2The pH value of precursor solution is 0~3, including a concentration of 0.02M
The MnO of~0.2M4 -；
S2. MnO will be attached with2Conductive substrates immerse in 0.34%~3.4% sugar juice and impregnate 1h~for 24 hours so that
Sugar juice, which is adsorbed on, is attached with MnO2Conductive substrates surface；
S3. it is attached with MnO by what the step S2 was obtained2Conductive substrates it is fully dry, and 400 DEG C in protective atmosphere
~1000 DEG C of heating 0.5h~3h so that the sugar charcoal in the sugar juice turns to amorphous carbon layer, while the MnO2It is reduced
The electrode is obtained, the manganese oxide particle is by 0%~38.5% in amorphous carbon layer for manganese oxide particle
Mn3O4Particle and 61.5%~100% MnO particles composition.
Preferably, the sugar in the sugar juice is disaccharide.
As it is further preferred that the disaccharide is glucose, sucrose, fructose or lactose.
Other side according to the invention additionally provides a kind of ultracapacitor, including above-mentioned cathode.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, due to Mn oxide
Particle can obtain following advantageous effect as negative material：
1, present invention selection is selected for the low disadvantage of current super capacitor anode capacity by Mn3O4Nano particle and
Active material of the manganese and oxygen compound layer of MnO nano particles composition as cathode, verified, specific capacity may be up to 662.9F/
G improves 50% or more than the prior art；
2, the cyclical stability that manganese oxide particle is improved using amorphous carbon layer is slowed down material and occurred in cycle charge-discharge
Material dissolving, improve the cycle life of cathode, after cycle charge-discharge 3000 times, original state that specific capacity still maintains
Under about 100%；
3, manganese and oxygen compound particle is to grow and the method for non-adhesive is combined with conductive substrates, to increase leading for cathode
Electrically, the specific capacity and rate capability of cathode are improved；
4, manganese and oxygen compound particle is generated using 400 DEG C~1000 DEG C of temperature, while generates amorphous carbon layer, ensured
The mechanical strength that conductive substrates are avoided while having enough active material MnO nano particles to generate declines and cathode is made to be easy to break
Rhegma is bad.
Description of the drawings
Fig. 1 is the scanning electron microscope diagram of comparative example 1 of the present invention；
Fig. 2 is carbon cloth and the X-ray diffractogram of comparative example 1-6；
Fig. 3 is the scanning electron microscope diagram of comparative example 1-6 of the present invention；
Fig. 4 is the cycle charge-discharge life diagram of comparative example 2-6 of the present invention；
Fig. 5 is the X-ray diffractogram of the embodiment of the present invention 1；
Fig. 6 is the scanning electron microscope diagram of the embodiment of the present invention 1；
Fig. 7 is the transmission electron microscope figure of the embodiment of the present invention 1；
Fig. 8 is area capacity of the embodiment of the present invention 1 under different current densities；
Fig. 9 is the cycle charge-discharge life diagram of the embodiment of the present invention 1.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
It does not constitute a conflict with each other and can be combined with each other.
The present invention provides a kind of ultracapacitor and for the cathode of the ultracapacitor, including conductive substrates, with
And it is grown on the amorphous carbon layer on conductive substrates surface, it is manganese oxide particle that grain size is embedded in the amorphous carbon layer, described
The mass ratio of manganese oxide particle and the amorphous carbon layer is 0.039:1~118:1, and preferably 6:1~20:1；
Wherein, collector of the conductive substrates as the cathode, material are carbon cloth, carbon fiber, nickel foam or not
Become rusty steel；And since carbon cloth has good flexibility and higher heat resisting temperature, to the material preferably as conductive substrates
Material；
The manganese oxide particle is for the active material as the cathode, by 0%~38.5% Mn3O4Particle with
And 61.5%~100% MnO particles form, wherein Mn3O4The grain size of particle is 3nm~40nm, and the grain size of MnO particles is
2nm~30nm；
The amorphous carbon layer is used to improve the cyclical stability of manganese oxide particle, and thickness is 2nm~300nm, and
Preferably 5nm~50nm；When amorphous carbon layer is excessively thin or the mass ratio of manganese oxide particle and the amorphous carbon layer is excessive
When, since manganese oxide particle lacks protection, and the stability of chemical property is affected, and the cycle life of cathode can be deteriorated；
, whereas if the ratio of manganese oxide particle reduces, then the redox reaction of Mn oxide is affected, the specific capacity of cathode
It can decline.
The preparation method of above-mentioned cathode, includes the following steps：
S1. under air-proof condition, conductive substrates are placed in MnO2In precursor solution, 85 DEG C~120 DEG C heating 15min~
360min, acquisition are attached with MnO2Conductive substrates, wherein the MnO2MnO including sheet2And linear MnO2；It is described
MnO2The pH value of precursor solution is 0~3, includes the MnO of a concentration of 0.02M~0.2M4 -；
S2. MnO will be attached with2Conductive substrates immerse in 0.34%~3.4% sugar juice and impregnate 1h~for 24 hours so that
It is described to be attached with MnO2Conductive substrates, be attached with average quality be 0.00034g/m2~0.034g/m2Sugar, sugar juice it is dense
Du Taigao can make the quality of the sugar of attachment become more, cause the specific capacity of electrode to decline to which amorphous carbon layer is blocked up, on the contrary
Then lead to that amorphous carbon layer is excessively thin and influences its cyclical stability；The sugar is disaccharide, such as glucose, sucrose, fructose or breast
Sugar, and wherein, it, will not be with MnO since sucrose is nonreducing sugar2It reacts and is more easy to control preparation condition, because
This ingredient preferably as sugar juice；
S3. it is attached with MnO by what the step S2 was obtained2Conductive substrates drying after in protective gas (such as pure nitrogen gas, argon
Gas etc.) under heat 0.5h~3h so that the MnO2It is reduced to Mn3O4The Mn oxide of particle and MnO particles composition
Grain, while the sugar charcoalization forms amorphous carbon layer, obtains the electrode；
Heating temperature is higher, and the ratio for restoring MnO particles in the manganese oxide particle of generation is bigger, meanwhile, Mn oxide
The grain size of particle is with regard to smaller, and to which opposite specific surface area is bigger, electro-chemical activity point relative increase, the specific capacity of cathode can be got over
Greatly, however excessively high temperature may cause the mechanical performance of conductive substrates to decline, therefore heating temperature need to be at 400 DEG C~1000 DEG C
Between, heating time can be reduced when temperature is high in right amount.
Comparative example 1
Carbon cloth is successively cleaned by ultrasonic 10min with acetone, ethyl alcohol, water, takes out and is immersed in ultrasound 5min in 20ml concentrated hydrochloric acids.
By 1mmol potassium permanganate, 0.5ml concentrated hydrochloric acids are dissolved in the deionized water of 35ml, obtain a concentration of 29mM, and pH value is 0.7
MnO2Precursor solution；
Carbon cloth is immersed into MnO2In precursor solution, and it is transferred to autoclave liner, is put into 85 DEG C of baking ovens respectively
React 2h.Reaction terminates to naturally cool to room temperature, takes out sample and is cleaned 3 times with deionized water, 40 DEG C of vacuum drying 6h are obtained
MnO2/ carbon cloth sample, as a comparison case 1.
Comparative example 2
By the MnO of comparative example 12/ carbon cloth sample, which connects, to be put into tube furnace, and high-purity N is passed through with the flow of 500sccm2+ 10%
H2Hereafter tube furnace is warming up to 200 DEG C by about 30min respectively, and in the high-purity N of 150sccm2+ 10%H2Middle heat preservation 1h.Reaction
End naturally cools to room temperature, takes out sample.As a comparison case 2.
Comparative example 3
Comparative example 2 is repeated with the same steps, difference lies in the temperature of heat preservation is 300 DEG C.
Comparative example 4
By the MnO of comparative example 12/ carbon cloth sample is directly placed into tube furnace, and high-purity N is passed through with the flow of 500sccm2About
Hereafter tube furnace is warming up to 200 DEG C by 30min respectively, and in the high-purity N of 150sccm2Middle heat preservation 1h.It is cold that reaction terminates nature
But room temperature is arrived, sample is taken out.
Comparative example 5
Comparative example 4 is repeated with the same steps, difference lies in the temperature of heat preservation is 300 DEG C.
Comparative example 4
Comparative example 4 is repeated with the same steps, difference lies in the temperature of heat preservation is 400 DEG C.
Comparative example 5
Comparative example 4 is repeated with the same steps, difference lies in the temperature of heat preservation is 500 DEG C.
Comparative example 6
Comparative example 4 is repeated with the same steps, difference lies in the temperature of heat preservation is 600 DEG C.
Embodiment 1
S1. it using carbon cloth as conductive substrates, successively uses acetone, ethyl alcohol, water to be cleaned by ultrasonic carbon cloth 10min, takes out and impregnate
The ultrasound 5min in 20ml concentrated hydrochloric acids, as flexible substrate.By 1mmol potassium permanganate, 0.5ml concentrated hydrochloric acids are dissolved in going for 35ml
In ionized water, a concentration of 29mM, the MnO that pH value is 0.7 are obtained2Precursor solution；
Carbon cloth is immersed into MnO2In precursor solution, and it is transferred to autoclave liner, is put into 85 DEG C of baking ovens respectively
React 2h.Reaction terminates to naturally cool to room temperature, takes out sample and is cleaned 3 times with deionized water, 40 DEG C of vacuum drying 6h are obtained
MnO2/ carbon cloth sample；
S2.3.42g sucrose is dissolved in 100ml deionized waters, a concentration of 3.4% sugar juice is obtained, by MnO2/ carbon cloth
Sample is immersed in 12h in the solution, takes out sample and in 80 DEG C of dry 2h；
S3. by MnO2/ carbon cloth sample is placed in tube furnace, and first lead to flow in tube furnace enters high-purity N for 500sccm2
As protective gas about 30min, hereafter tube furnace is heated up respectively 600 DEG C, and in the high-purity N of 150sccm2Middle heat preservation 1h.Instead
It should terminate to naturally cool to room temperature, take out sample, obtain cathode.
To simplify the description, the preparation condition of embodiment 2- embodiments 8 is classified as table 1.
The preparation condition of 1 embodiment 2- embodiments 8 of table
Analysis of experimental results
Fig. 1 is the scanning electron microscope diagram of comparative example 1 of the present invention, it can be seen that MnO2Nanometer sheet is uniformly grown in
Carbon cloth surfaces.
Fig. 2 is carbon cloth and the X-ray diffractogram (JCPDS 80-1098) of comparative example 1-6, it can be seen that carbon cloth surfaces are given birth to
Long δ-MnO2.With the raising of temperature, δ-MnO2It is gradually converted into Mn3O4(JCPDS 089-4837) and MnO (JCPDS
078-0424) the mixed phase of two kinds of substances.Fig. 3 a-f indicate the scanning electron microscope diagram of comparative example 1-6 of the present invention successively, can
To find out, when tube furnace is warming up to 400 DEG C~600 DEG C, MnO2Nanometer sheet pattern gradually becomes the pattern of nano particle.Manganese oxygen
Compound particle and the amorphous carbon layer that thickness is 2nm~20nm, the manganese oxide particle include that grain size is 2nm~30nm
Nano particle.
Fig. 4 is comparative example 2-6 of the present invention in 10mA/cm2Cycle charge-discharge life diagram under constant current charge-discharge；It can see
Go out, with the raising of holding temperature, due to MnO2Generate more MnO, MnO2The area capacity and cycle of/carbon cloth electrode are steady
Qualitative raising, when annealing temperature is 600 DEG C, MnO2/ carbon cloth electrode performance reaches best.
Fig. 5 is the X-ray diffractogram of the embodiment of the present invention 1；As can be seen that product is pure MnO (JCPDS 075-
0626), not any other impurity peaks are measured, and the peak of wherein carbon comes from carbon cloth
Fig. 6 is the scanning electron microscope diagram of the embodiment of the present invention 1；It can be seen that embodiment 1 maintains and 1 class of comparative example
As structure, show MnO2/ carbon cloth sample is immersed in the maintenance for being conducive to nanostructure in sucrose solution before annealing.
Fig. 7 is that the TEM of the embodiment of the present invention 1 schemes, and can see that the nanometer sheet on 1 surface of embodiment is amorphous carbon, amorphous
Carbon is as holder by MnO2The MnO nano particles insertion that reduction generates so that nanometer sheet remains on and MnO2Nanometer sheet is similar
Pattern.
The specific capacity that can be seen that embodiment 1 in Fig. 8 is up to 662.9F/g, than in the prior art Mn3O4The specific volume of material
Amount improves 50% or more, is more applicable for such as hybrid-electric car, and the high energy in the equipment such as all-electric automobile is asymmetric super
The negative material of capacitor.
3000 (10mA/cm of Fig. 9 cycle charge-discharges2Constant current charge-discharge) after the initial capacity 100% still maintained,
It is 91% compared to the initial capacity maintained after Fig. 7 cycle charge-discharges 2000 times, ring stability tool improves a lot.
Above-mentioned detection is carried out to embodiment 2-8, also can get result similar to Example 1；Simultaneously as can be seen that implementing
The electrode that example 1-8 is obtained includes the amorphous carbon layer that conductive substrates and thickness are 2nm~200nm successively from bottom surface to top surface,
Mn is embedded in amorphous carbon layer3O4Particle and MnO particles, wherein the grain size of MnO particles is 2nm~30nm, and mass fraction is big
In 61.5%, Mn3O4The grain size of particle is 3nm~40nm, Mn3O4The manganese oxide particle and institute of particle and MnO particles composition
The mass ratio for stating amorphous carbon layer is about 0.039:1~118:1, when the mass ratio of manganese oxide particle and the amorphous carbon layer
It is 6:1~20:When 1, the specific capacity and cyclical stability of embodiment have preferable performance.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all within the spirits and principles of the present invention made by all any modification, equivalent and improvement etc., should all include
Within protection scope of the present invention.
Claims (8)
1. a kind of cathode for ultracapacitor, which is characterized in that including conductive substrates, and be grown on conductive substrates surface
Amorphous carbon layer, embedded with the manganese oxide particle that grain size is 2nm~40nm, the amorphous carbon layer in the amorphous carbon layer
Thickness be 2nm~300nm, the manganese oxide particle by 0%~38.5% Mn3O4Particle and 61.5%~100%
MnO particles form, and the mass ratio of the manganese oxide particle and the amorphous carbon layer is 0.039:1~118:1.
2. cathode as described in claim 1, which is characterized in that the conductive substrates are carbon cloth, carbon fiber, nickel foam or stainless
Steel.
3. cathode as described in claim 1, which is characterized in that the Mn3O4The grain size of particle is 3nm~40nm, the MnO
The grain size of particle is 2nm~30nm.
4. cathode as described in claim 1, which is characterized in that the thickness of the amorphous carbon layer is 5nm~50nm.
5. cathode as described in claim 1, which is characterized in that the quality of the manganese oxide particle and the amorphous carbon layer
Than being 6:1~20:1.
6. the preparation method of the cathode as described in any one of claim 1-5, which is characterized in that include the following steps：
S1. under air-proof condition, conductive substrates are placed in MnO2In precursor solution, 85 DEG C~120 DEG C heating 15min~
360min, acquisition are attached with MnO2Conductive substrates；The MnO2The pH value of precursor solution is 0~3, including a concentration of 0.02M
The MnO of~0.2M4 -；
S2. MnO will be attached with2Conductive substrates immerse in 0.34%~3.4% sugar juice and impregnate 1h~for 24 hours so that sugar juice
It is adsorbed on and is attached with MnO2Conductive substrates surface；
S3. it is attached with MnO by what the step S2 was obtained2Conductive substrates it is fully dry, and 400 DEG C in protective atmosphere~
1000 DEG C of heating 0.5h~3h so that the sugar charcoal in the sugar juice turns to amorphous carbon layer, while the MnO2It is reduced to
Manganese oxide particle, obtains the electrode, the manganese oxide particle by 0%~38.5% Mn3O4Particle and 61.5%~
100% MnO particles composition.
7. preparation method as claimed in claim 6, which is characterized in that the sugar in the sugar juice is glucose, sucrose, fructose
Or lactose.
8. a kind of ultracapacitor, which is characterized in that include the cathode as described in any one of claim 1-5.
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| CN103117175A (en) * | 2013-02-25 | 2013-05-22 | 中国科学院过程工程研究所 | Multi-element composite nano-material, preparation method thereof and application thereof |
| CN103440996A (en) * | 2013-08-30 | 2013-12-11 | 天津工业大学 | Method for preparing nanometer manganous-manganic oxide/carbon composite energy storage material |
| CN105551813A (en) * | 2016-01-26 | 2016-05-04 | 华中科技大学 | Preparation method of MnO2/porous carbon film/nickel composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103117175A (en) * | 2013-02-25 | 2013-05-22 | 中国科学院过程工程研究所 | Multi-element composite nano-material, preparation method thereof and application thereof |
| CN103440996A (en) * | 2013-08-30 | 2013-12-11 | 天津工业大学 | Method for preparing nanometer manganous-manganic oxide/carbon composite energy storage material |
| CN105551813A (en) * | 2016-01-26 | 2016-05-04 | 华中科技大学 | Preparation method of MnO2/porous carbon film/nickel composite material |
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