CN108922788A - A kind of PEDOT@Na3(VOPO4)2F composite material, preparation method and its application - Google Patents
A kind of PEDOT@Na3(VOPO4)2F composite material, preparation method and its application Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/04—Hybrid capacitors
- H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- 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 present invention provides PEDOT@Na3(VOPO4)2F composite material, preparation method and its application, the composite material are mixed by the way that sodium source, vanadium source, Fluorine source and phosphate is added, and are carried out lithium, calcination processing at hydro-thermal and are obtained pure phase Na3(VOPO4)2After F, then in-situ polymerization coats polyethylene dioxythiophene（PEDOT）It can be obtained, method is simple and efficient, and is easy to expand large-scale production.Utilize the PEDOT@Na3(VOPO4)2F composite material is " rocking chair " formula sodium ion capacitor made of anode, and operating voltage is high, has extended cycle life, and specific energy is much higher than general electrochemical capacitor, up to 158 Wh kg−1More than, specific power density is up to 7000 W kg−1, there is very high practical value.
Description
Technical field
The present invention relates to nano material preparation and energy field, specifically a kind of PEDOT@Na3(VOPO4)2F composite material
Preparation method and with the material be positive " rocking chair " formula sodium ion capacitor.
Background technique
With the fast development of the extensive energy storage including smart grid and its to high power density, high-energy density
The demand of energy storage device combines the lithium-ion capacitor of both double layer capacitor and lithium ion battery advantage by people
Extensive concern.But lithium resource is similar with petroleum, is a kind of scarce resource, and the reserves in the earth's crust are limited, and point in the whole world
Cloth is uneven, largely limits its application in extensive energy storage.In contrast, it with the sodium of the same main group of lithium, provides
Source is abundant, cheap, and has similar physics, chemical property, and sodium ion capacitor right and wrong are often with the storage for having development potentiality
Energy system, is increasingly becoming the research hotspot in electrochemical energy storage field.Similar with lithium-ion capacitor, sodium ion capacitor is usually adopted
With cell type negative electrode material and electric double layer type positive electrode, so that sodium ion capacitor possesses sodium-ion battery and double electricity simultaneously
The double dominant of layer capacitor has power density more higher than sodium-ion battery, while having again higher than double layer capacitor
Energy density.Therefore sodium ion capacitor is expected to used in high-energy such as electric car, electrical equipment and aerospace facilities, greatly
The extensive energy storage field of power-type.
V2O5And Na2Ti3O7Equal stratified materials have been applied to sodium ion capacitor anode material.Chinese Academy of Sciences Changchun
The Na of the reports such as applied chemistry study institute Wang Hongyu2Ti3O7//AC sodium ion capacitor, energy density is up to 34Wh kg-1It (is based on
Positive and negative anodes active material quality).This conventional sodium ion capacitor sodium ion in charging is embedded into battery-type negative electrode, simultaneously
Anion can be adsorbed onto anode.That is based on electrolyte consumption mechanism, i.e., the energy storage mechanism of conventional sodium ion capacitor is
Electrolyte zwitterion separates during the charging process, thus capacitor internal resistance is caused to increase.To solve this problem, it needs using big
The electrolyte of amount.This reduces the specific energy densities of sodium ion capacitor integral device.
In order to further increase the specific energy density of sodium ion capacitor, it is necessary to improve the knot of traditional sodium ionistor
Structure, can using the positive electrode of cell type and the negative electrode material of electric double layer type, that is, develop a kind of novel " rocking chair " formula sodium from
Sub-capacitor.When charging, sodium ion is deviate from from battery-type positive electrode material, is adsorbed onto capacitive negative electrode material surface；When electric discharge,
Sodium ion is embedded into positive electrode from negative electrode material surface desorption.The energy storing structure of this " rocking chair " formula only need with it is secondary
The comparable a small amount of electrolyte of battery can work normally.In general, design prepares the excellent cell type material of high rate performance
It is the key that obtain high-performance sodium ion capacitor.In general, the high rate performance and cyclical stability of battery-type electrode chose material are poor,
It is bad to result in the sodium ion capacitor cycle service life.Therefore, there is stable structure, high-energy density and fast charging and discharging ability
Positive electrode needs to be researched and developed.Currently used storage sodium positive electrode has stratiform transition metal oxide, polyanionic
Close object, Prussian blue similar object etc..Wherein polyanionic compound, transition metal phosphate material especially therein, by
It is that one kind is having promising storage sodium just very much in the ion channel with Three-dimensional Open, high structural stability and thermal stability
Pole material.The Na of NASICON (Na super ionic conductor) structure3V2(PO4)3It is considered as a kind of important storage
Sodium positive electrode, voltage platform can participate in deintercalation in 3.4V or so there are two Na, and corresponding theoretical capacity is 117mAh g-1。
The Na of tetragonal3V2(PO4)2F3Also can 2 Na of reversible deintercalation, voltage platform is about 3.9V, and theoretical capacity is 128mAh g-1, and F therein can be replaced by O, form a series of Na3(VO1-xPO4)2F1+2xThe introducing of (0 >=x >=1), O can be improved
The diffusion rate of sodium ion, wherein Na3(VOPO4)2F operating potential with higher, best high rate performance, energy density is most
High reachable 600Wh kg-1.But the electron conduction of the material is not high, limits further increasing for its chemical property.And it leads
Electric polymer PEDOT material has the characteristics that molecular structure is simple, conductivity is high, is easily-synthesized, environmental stability is good, therefore prepares
The Na of PEDOT cladding3(VOPO4)2F composite material can be effectively improved Na3(VOPO4)2The chemical property of F material.
Summary of the invention
In order to solve existing technical problem, the purpose of the present invention is to provide a kind of PEDOT Na3(VOPO4)2F is compound
Material is nanostructure, can effectively shorten the transmission range of ion and electronics, increase the specific surface area of electrochemical material
Be conducive to the abundant infiltration of electrolyte, while the cladding of conducting polymer PEDOT improves the electric conductivity of material entirety again.
It is yet a further object of the present invention to provide one kind with PEDOT@Na3(VOPO4)2F composite material is positive " shakes
Chair " formula sodium ion capacitor, operating voltage is high, has extended cycle life, and specific energy is much higher than general electrochemical capacitor, reachable
158Wh kg-1More than, specific power density is up to 7000W kg-1, there is very high practical value.
In order to achieve the above-mentioned object of the invention, present invention employs technical solutions below：
A kind of PEDOT@Na3(VOPO4)2F composite material, conducting polymer PEDOT are coated on Na3(VOPO4)2F outer layer, it is whole
Body is nano cubic box-shaped structure, is evenly distributed, and side length is 200~500nm.
PEDOT@Na3(VOPO4)2The preparation method of F composite material, steps are as follows：
(1), by oxalic acid and V2O5It is separately added into water, 70 DEG C continue stirring until to obtain blue clear solution, add phosphoric acid
Salt, Na2CO3And NaF, continue stirring 30 minutes；PH to 7 is adjusted with ammonium hydroxide, then carries out hydro-thermal reaction；Obtained solid filtering point
From, washing, dry, then calcining obtains pure phase Na3(VOPO4)2F powder (Advanced Materials 29 (2017)
1701968(High-Energy/Power and Low-Temperature Cathode for Sodium-Ion
Batteries:In Situ XRD Study and Superior Full-Cell Performance))。
Its mesoxalic acid, V2O5、PO4 3-、Na2CO3Molar ratio with NaF is 3：1：2：1：1；
The phosphate is ammonium phosphate, diammonium hydrogen phosphate or ammonium dihydrogen phosphate；
The temperature of hydro-thermal reaction is 180 DEG C, and the time is 12~36h；
Dry to be dried in vacuo, drying temperature is 60~100 DEG C, and drying time is 6~12h.
Calcination atmosphere is nitrogen or argon gas, and calcination temperature is 400~700 DEG C, and soaking time is 3~12h, heating rate
For 1~3 DEG C of min-1。
(2), powder obtained in step 1) is distributed to the hydrochloric acid solution (pH containing 3,4- ethene dioxythiophene (EDOT)
=1) in, ammonium persulfate is added, stirs 10h, centrifugation, PEDOT@Na can be obtained in 60 DEG C of vacuum drying 12h3(VOPO4)2F is multiple
Condensation material.
The quality of EDOT is Na3(VOPO4)2The 10%~50% of F mass, the quality of ammonium persulfate be EDOT mass 1~
5 times.
A kind of " rocking chair " formula sodium ion capacitor, the positive electrode of capacitor are PEDOT@Na3(VOPO4)2F composite material,
Negative electrode material is absorbent charcoal material.Anode utilizes the insertion and abjection energy storage of sodium ion, and cathode is stored up using the adsorption desorption of sodium ion
Energy.Sodium ion is deviate from from anode when charging, while sodium ion is adsorbed on cathode.When electric discharge in contrast." rocking chair " formula
The quality of active material is with positive active material and than being 1 in the negative electrode material of sodium ion capacitor：1.5.
Beneficial effect：
(1) simple production process of composite material prepared by the present invention is easy to expand large-scale production, and microscopic appearance is nanometer
Cube box-shaped structure, is evenly distributed, and side length is 200~500nm.
(2) the PEDOT@Na that the present invention obtains3(VOPO4)2The structure of F composite material, nanosizing can effectively shorten
The transmission range of ion and electronics, the specific surface area for increasing electrochemical material are conducive to the abundant infiltration of electrolyte, lead simultaneously
The cladding of electric polymer PEDOT improves the electric conductivity of material entirety again.
(3) present invention uses PEDOT@Na for the first time3(VOPO4)2F composite material is battery-type positive electrode material, is with active carbon
Electric double layer capacitance type negative electrode material, " rocking chair " formula sodium ion capacitor performance being assembled into is excellent, and operating voltage is high, recycles the longevity
Life is long, and (86.6%) 1000 circulations, capacity retention ratio are greater than, and specific energy is much higher than general electrochemical capacitor, reachable
158Wh kg-1More than, there is very high practical value.
Detailed description of the invention
Fig. 1 is PEDOT@Na prepared by the embodiment of the present invention 13(VOPO4)2The SEM of F composite material schemes；
Fig. 2 is PEDOT@Na prepared by the embodiment of the present invention 13(VOPO4)2The XRD diagram of F composite material；
Fig. 3 is PEDOT@Na prepared by the embodiment of the present invention 13(VOPO4)2F composite material in 0.1C (1C=120mA
g-1, similarly hereinafter) and charging and discharging curve figure under current density；
Fig. 4 is the assembling of the embodiment of the present invention 1 with PEDOT@Na3(VOPO4)2F composite material is anode, with active raw material of wood-charcoal
Material is charging and discharging curve figure of " rocking chair " the formula sodium ion capacitor of cathode under 1C current density；
Fig. 5 is the assembling of the embodiment of the present invention 1 with PEDOT@Na3(VOPO4)2F composite material is anode, with active raw material of wood-charcoal
Material is circulation 1000 time life curve figure of " rocking chair " the formula sodium ion capacitor of cathode under 10C current density；
Fig. 6 is the assembling of the embodiment of the present invention 1 with PEDOT@Na3(VOPO4)2F composite material is anode, with active raw material of wood-charcoal
Material is that energy density-power density (quality based on positive and negative anodes active material) of " rocking chair " formula sodium ion capacitor of cathode is bent
Line (Ragone curve) figure.
Specific embodiment
The present invention will be further explained below with reference to the attached drawings.
Above content of the invention is described in further detail below by way of specific embodiment.But this should not be understood
Following examples are only limitted to for the contents of the present invention.
Embodiment 1
PEDOT@Na3(VOPO4)2The preparation method of F composite material, steps are as follows：
Step (1), pure phase Na3(VOPO4)2The preparation of F powder：By 6mmol oxalic acid and 2mmol V2O5It is separately added into 30mL
In water, 70 DEG C continue stirring until to obtain blue clear solution, add 4mmol ammonium dihydrogen phosphate, 2mmol Na2CO3And 2mmol
NaF continues stirring 30 minutes, and ammonium hydroxide is added to adjust pH to 7, and then 180 DEG C of hydro-thermals for 24 hours, are separated by filtration, wash, and 80 DEG C of vacuum are dry
Dry 6h.
Pure phase Na will be obtained after the lower 500 DEG C of calcinings 4h of gained powders A r3(VOPO4)2F powder, heating rate are 1 DEG C of min-1；
Step (2), PEDOT@Na3(VOPO4)2The preparation of F composite material：By the Na of 200mg3(VOPO4)2F, which is distributed to, to be contained
Have and stir 30min in the hydrochloric acid solution (pH=1) of the 3,4-rthylene dioxythiophene (EDOT) of 50 μ L, 100mg ammonium persulfate is added,
10h, centrifugation are stirred, final PEDOT@Na can be obtained in 60 DEG C of vacuum drying 12h3(VOPO4)2F composite material.
Fig. 1 is PEDOT@Na prepared by the present invention3(VOPO4)2The SEM of F composite material schemes；
Fig. 2 is PEDOT@Na prepared by the present invention3(VOPO4)2The XRD diagram of F composite material；
It is not difficult to find out by above-mentioned attached drawing, the PEDOT@Na that the present embodiment obtains3(VOPO4)2F composite material is nanometer box
Structure, even size distribution, side length are 200~500nm, and XRD diagram shows that gained sample is the Na of NASICON structure3(VOPO4)2F。
With 7:2:1 mass ratio weighs the resulting PEDOT@Na of the present embodiment respectively3(VOPO4)2F material, acetylene black and
Binder Kynoar, using N-Methyl pyrrolidone as solvent, is sufficiently stirred into paste, then uses film after grinding uniformly
Machine is evenly coated on copper foil, and sufficiently dry 12h, is cut into the electrode slice of suitable size at 110 DEG C.The group of half-cell is filled with metal
Sodium is cathode, uses glass fibre membrane for diaphragm, with 1M NaPF6EC/PC (volume ratio 1:1) it is electrolyte, is being full of argon
It is assembled into button cell in the glove box of gas, charge-discharge test is then carried out on Land battery test system.
The PEDOT@Na obtained of embodiment 1 measured3(VOPO4)2F composite material is in 0.1C (1C=120mA g-1) electricity
Charging and discharging curve under current density is as shown in Figure 3.Reversible capacity is close to 120mAh g-1。
The assembling of " rocking chair " formula sodium ion capacitor is similar with the assembling of half-cell, only cathode using active carbon,
Mixture (the mass ratio 7 of acetylene black and binder:2:1).What electrolyte was selected is the electrolyte as half-cell.Just
The matching of the negative electrode material performance influence final on ionistor is very big, and according to the formula of charge conservation, this patent is excellent
The positive active material of choosing and the mass ratio of negative electrode active material are 1.5.It should be noted that before the assembling of sodium ion capacitor,
Cathode needs in half-cell in advance in 100mA g-11 circle of circulation under current density.
The embodiment 1 measured is obtained with PEDOT@Na3(VOPO4)2F composite material be positive " rocking chair " formula sodium from
Sub-capacitor is in 1C current density (based on PEDOT@Na in anode3(VOPO4)2Charging and discharging curve under the quality of F, similarly hereinafter) is such as
Shown in Fig. 4.In the cycle life curve under 10C current density as shown in figure 5, capacity retention ratio is after circulation 1000 times
86.6%.Fig. 6 is energy density-power density curve (Ragone curve) of the sodium ion capacitor.As can be seen from the figure
" rocking chair " formula sodium ion capacitor energy density and the power density (matter based on positive and negative anodes active material that this patent assembles
Amount) it is up to 158.8Wh kg respectively-1With 7000W kg-1。
The reaction condition that embodiment 2-5 is related to step 2 is as shown in table 1：
Table 1
| Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| MEDOT/MNa3(VOPO4)2F* 100% | 10% | 20% | 40% | 50% |
| M ammonium persulfate/MEDOT | 1.5 | 1.5 | 1.5 | 1.5 |
| Reversible specific capacity (mAhg-1) | 115.1 | 116.8 | 112.3 | 110.2 |
It seen from table 1, is Na in the quality that EDOT is added3(VOPO4)2In 10%~50% range of F mass, in 0.1C
Under current density, reversible specific capacity experienced the process of from low to high, illustrate on the one hand the cladding of PEDOT improves composite wood
The electron conduction of material, on the other hand too thick PEDOT clad can also hinder the transmission of sodium ion.
There are many concrete application approach of the present invention, the above is only a preferred embodiment of the present invention, it is noted that for
For those skilled in the art, without departing from the principle of the present invention, it can also make several improvements, this
A little improve also should be regarded as protection scope of the present invention.
Claims (6)
1. a kind of PEDOT@Na3(VOPO4)2F composite material, which is characterized in that conducting polymer PEDOT is coated on Na3
(VOPO4)2F outer layer, generally nano cubic box-shaped structure, are evenly distributed, and side length is 200~500nm.
2. PEDOT@Na described in claim 13(VOPO4)2The preparation method of F composite material, which is characterized in that steps are as follows：
(1), by oxalic acid and V2O5It is separately added into water, continues stirring until to obtain blue clear solution under heating state, add phosphorus
Hydrochlorate, Na2CO3And NaF, continue to be dispersed with stirring uniformly；Adjust pH to 7,180 DEG C of 12~36h of hydro-thermal reaction；Obtained solid filtering
Separation, washing, drying, then calcining obtains pure phase Na3(VOPO4)2F powder；
(2), powder obtained in step (1) is distributed in the hydrochloric acid solution containing 3,4-rthylene dioxythiophene, over cure is added
Sour ammonium stirs 10h, is centrifuged, and PEDOT@Na can be obtained in vacuum drying3(VOPO4)2F composite material.
3. PEDOT@Na as claimed in claim 23(VOPO4)2The preparation method of F composite material, it is characterised in that in step (1)：
Oxalic acid, V2O5、PO4 3-、Na2CO3Molar ratio with NaF is 3：1：2：1：1；
The phosphate is ammonium phosphate, diammonium hydrogen phosphate or ammonium dihydrogen phosphate；
Dry to be dried in vacuo, drying temperature is 60~100 DEG C, and drying time is 6~12h；
Calcination atmosphere is nitrogen or argon gas, and calcination temperature is 400~700 DEG C, and soaking time is 3~12h, heating rate 1
~3 DEG C of min-1。
4. PEDOT@Na as claimed in claim 23(VOPO4)2The preparation method of F composite material, it is characterised in that in step (2)：
The quality of EDOT is Na3(VOPO4)2The 10%~50% of F mass, the quality of ammonium persulfate are 1~5 times of EDOT mass, hydrochloric acid
The pH=1 of solution.
5. a kind of " rocking chair " formula sodium ion capacitor, which is characterized in that the positive electrode of capacitor is described in claim 1
PEDOT@Na3(VOPO4)2F composite material, negative electrode material are absorbent charcoal material；Anode is stored up using the insertion and abjection of sodium ion
Can, cathode utilizes the adsorption desorption energy storage of sodium ion；Sodium ion is deviate from from anode when charging, while sodium ion is adsorbed on cathode；
When electric discharge in contrast.
6. " rocking chair " formula sodium ion capacitor described in claim 5, it is characterised in that " rocking chair " the formula sodium ion capacitor
Cathode in active material quality and anode in active material mass ratio be 1：1.5.
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| CN110120512A (en) * | 2019-05-24 | 2019-08-13 | 陕西科技大学 | A kind of sheet EDOT@Cu3(PO4)2The preparation method of composite material |
| CN110247037A (en) * | 2019-06-11 | 2019-09-17 | 华中科技大学 | A kind of fluorophosphoric acid vanadium oxygen sodium/graphene complex and preparation method and purposes |
| CN113571706A (en) * | 2021-07-12 | 2021-10-29 | 常州大学 | PEDOT-coated secondary water system zinc ion battery positive electrode material and preparation method thereof |
| CN114613966A (en) * | 2022-03-23 | 2022-06-10 | 广州市虎头电池集团股份有限公司 | Honeycomb negative electrode material and preparation method thereof |
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| CN115642237A (en) * | 2022-10-28 | 2023-01-24 | 无锡零一未来新材料技术研究院有限公司 | Sodium ion composite cathode material and preparation method and application thereof |
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Application publication date: 20181130 |