CN109767925A - T-Nb for lithium ion super capacitor2O5/ egg white carbon composite and preparation method thereof - Google Patents
T-Nb for lithium ion super capacitor2O5/ egg white carbon composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of for lithium ion super capacitorT‑Nb2O5/ egg white carbon composite and preparation method thereof, niobic acid ammonium oxalic acid salt hydrate is added to the water, it is added in egg white after stirring, continue agitating solution to milky after dilute hydrochloric acid is added dropwise, hydro-thermal reaction is freeze-dried after filtering, then anneals in nitrogen atmosphere, last cleaned, dry, grinding, obtains the electrode material.The material can effectively alleviate Nb2O5The stacking of nanoparticle is reunited, to increase the effective ratio area of material and the utilization rate of active material；The carbon material generated after egg white high annealing rich in nitrogen oxygen element can be improved the wetability and electric conductivity of composite material；Porous structure may advantageously facilitate ion and quickly transmit and spread in electrode interior, to improve the high rate performance and cyclical stability of electrode material.
Description
Technical field
The present invention relates to lithium ion super capacitor electrode material technical fields, and in particular to one kind is used for lithium ion super
Capacitor it is porousT-Nb2O5/ egg white carbon composite electrode material and preparation method.
Background technique
Due to the urgent need to renewable and clean energy resource, electrochemical energy storage equipment is concerned and is widely ground
Study carefully.In all electrochemical energy storage facilities, supercapacitor and lithium ion battery are that two kinds of energy by favor is deposited
Storage system.Supercapacitor (double layer capacitor) has higher by charge adsorption/desorption of electrode surface fast and stable
Power density, but the specific surface area for being limited to electrode material causes its energy density usually lower.For lithium ion battery, by
It can be embedded into lithium ion to generate higher energy density inside electrode material, but slower lithium ion diffusion kinetics are led
Cause its power density and cycle life unsatisfactory.Lithium ion super capacitor (LISC) is that a kind of promising energy storage is set
It is standby, the advantage of supercapacitor and lithium ion battery can be made full use of.In simple terms, LISC be by support Rapid reversible lithium from
Son insertion/it is embedding go out characteristic battery-type positive electrode material and show charge adsorption desorption performance capacitive negative electrode material assembling and
At.Under the synergistic effect of two kinds of capacitor storage mechanisms, power density, energy density and the cycle life of LISC is obtained obviously
Improvement.However, the overall performance of LISC is limited to the slower redox reaction of battery-type electrode chose, so that power density has
Limit.Therefore, for the LISC of establishment very-high performance, it is extremely heavy for finding and develop the electrode material of promising high rate capability
It wants.
Nb2O5Because its theory capacitor is up to 200 mAh/g, while can occur with the lithium ion of electrode surface reversible counterfeit
Capacitance reaction and generate higher power density and be concerned.Its unique lithium ion fake capacitance characteristic can ensure Nb2O5It gathers around
There is outstanding dynamics-lithium ion that can quickly be embedded in electrode material without generating any crystal transition, to have preferable
Cyclical stability.However, Nb2O5The application of electrode is limited to its lower electric conductivity and ion diffusion rates.In recent years, it studies
Persons are made that a large amount of effort to overcome these difficulties, such as composite conducting material, doping heterogeneous element and nanosizing structure are set
Meter etc..However, these synthetic methods have the following problems: the inefficient usability of harsh experiment synthesis condition, the source Nb presoma
And special ancillary equipment.Therefore, it finds efficient, simple method and synthesizes nanostructure Nb2O5And Nb2O5Composite material is still
Face lot of challenges.
Summary of the invention
The object of the present invention is to provide a kind of for the porous of lithium ion super capacitorT-Nb2O5/ egg white carbon electrode material
And preparation method.
In order to solve the above technical problems, the present invention provides described porousT-Nb2O5The preparation side of/egg white carbon electrode material
Method, this method are by niobic acid ammonium oxalic acid salt hydrate (C4H4NNbO9·xH2O；99.99%) it is placed in egg white and carries out hydro-thermal reaction,
It is freeze-dried after filtering, then anneals in nitrogen atmosphere, last cleaned, dry, grinding obtains super for lithium ion
Grade capacitor it is porousT-Nb2O5/ egg white carbon electrode material, the specific steps are as follows:
1) egg white pre-processes: yolk being removed, after mixing evenly for use.
2) by niobic acid ammonium oxalic acid salt hydrate (C4H4NNbO9·xH2O；99.99%) it is add to deionized water, after stirring
It is added in egg white, continues agitating solution to milky after dilute HCl is added dropwise.
3) 20~24 h of hydro-thermal reaction at 180~200 DEG C naturally cools to filtering, freeze-drying after room temperature, obtains
Mixture.
4) 700~800 DEG C under nitrogen atmosphere, are warming up to the heating rate of 2~5 DEG C/min, 2~4 h of constant temperature is obtained
Combination product.
5) it is cleaned for several times with deionized water and dehydrated alcohol, is ground after dry repeatedly, obtain lithium ion super capacitor use
It is porousT-Nb2O5/ egg white carbon electrode material.
Further, niobic acid ammonium oxalic acid salt hydrate is add to deionized water in the ratio of 0.2g:10 mL, first will
It is in order to which niobic acid ammonium oxalic acid salt hydrate is dispersed in deionization that niobic acid ammonium oxalic acid salt hydrate, which is add to deionized water,
In water, if directly added it in egg white, since egg white viscosity is larger, even if stirring can not ensure that it is dispersed in
In egg white.The ratio provided is to ensure that niobic acid ammonium oxalic acid salt hydrate energy is fully dispersed in deionized water, ratio too Gao Buneng
Achieve the purpose that fully dispersed, ratio is too low to dilute egg white concentration, unfavorable to the chemical property for ultimately forming compound.
Further, niobic acid ammonium oxalic acid salt hydrate and the adding proportion of egg white are 0.2g:60 mL, niobic acid ammonium oxalates
Hydrate is niobium source, and egg white is carbon source, and ratio is too high, and final product carbon content is few, and electric conductivity is bad, Nb2O5Nanoparticle accumulation
Reunite；Ratio is too low, and final product content of niobium is low, and chemical property is bad.
Further, continue 30 min of agitating solution to milky after the dilute HCl of 0.5 mL, 2 mol/L is added dropwise, be added dropwise suitable
When the dilute hydrochloric acid of concentration advantageously forms the Nb of the orthorhombic phase crystal form of high energy-storage property2O5, concentration is too high, and amount of by-products increases, electricity
Chemical property is bad.
Further, hydro-thermal reaction of the present invention be in egg white lotion, it is anti-with 180~200 DEG C of target temperature
Answer 20~24 h.It is proved through repetition test, suitable target temperature and reaction time, is conducive to Nb2O5Nanoparticle is uniformly distributed
In egg white, it help to obtain the better composite material of performance and higher yield.
Further, when annealing, 700~800 DEG C are warming up to the heating rate of 2~5 DEG C/min, rear 2~4 h of constant temperature.
Annealing temperature is conducive to generate at 700~800 DEG C the Nb of orthorhombic phase crystal form2O5(T-Nb2O5).Suitable heating rate and constant temperature
Time is conducive to the generation of porous carbon ball and ensuresT-Nb2O5Nanoparticle is evenly distributed in carbon ball, to improve raw material
Utilization rate.
Further, the product obtained after annealing deionized water and dehydrated alcohol are washed down repeatedly, are then dried,
Last grind into powder can be used as electrode active material.It can remove the pairs such as the organic matter being present in product with dehydrated alcohol
Product, to improve the capacitive property of composite material.
Compared with prior art, the beneficial effects of the present invention are:
1) source egg white hydro-thermal process Nb can effectively alleviate Nb2O5The stacking of nanoparticle is reunited, to increase having for material
Imitate the utilization rate of specific surface area and active material.
2) after the egg white high annealing rich in nitrogen oxygen element the carbon material that generates can be improved composite material wetability and
Electric conductivity.
3) egg white is as biomass, abundance, renewable, environmental-friendly, is by simple, green treatment process
It can be made porousT-Nb2O5/ egg white carbon material, be used as electrode material has preferable capacitive character in lithium ion super capacitor
Energy.
4) preparation process of the present invention is simple, green, can effectively reduce the production cost of electrode material, enhances environmental-friendly
Property.
Detailed description of the invention
Fig. 1 is the porous of embodiment reed filmT-Nb2O5The SEM of/egg white carbon material schemes.
Fig. 2 is the porous of embodiment preparationT-Nb2O5The TEM of/egg white carbon material schemes.
Fig. 3 is the porous of embodiment preparationT-Nb2O5The HRTEM of/egg white carbon material schemes.
Fig. 4 is the porous of embodiment preparationT-Nb2O5The XRD spectra of/egg white carbon material.
Fig. 5 is the porous of embodiment preparationT-Nb2O5The TGA of/egg white carbon material schemes.
Fig. 6 is the porous of embodiment preparationT-Nb2O5The XPS spectrum figure of/egg white carbon material.
Fig. 7 is the porous of embodiment preparationT-Nb2O5The cyclic voltammetry curve figure of/egg white carbon electrode material.
Fig. 8 is the porous of embodiment preparationT-Nb2O5The specific volume spirogram of/egg white carbon electrode material under different current densities.
Fig. 9 is the porous of embodiment preparationT-Nb2O5The constant current charge-discharge curve graph of/egg white carbon electrode material.
Figure 10 is the porous of embodiment preparationT-Nb2O5The specific capacity of/egg white carbon electrode material with cycle-index variation
Figure.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention more comprehensible, with reference to embodiments to the present invention into
Row explains in detail.
The present invention with niobium oxalate is the source Nb, egg white is the source C, and by hydro-thermal-, that annealing two-step method can prepare rich nitrogen is porousT-Nb2O5/ egg white carbon composite.This material can effectively alleviate Nb2O5The stacking of nanoparticle is reunited, to increase
The effective ratio area of material and the utilization rate of active material；The carbon material generated after egg white high annealing rich in nitrogen oxygen element
It can be improved the wetability and electric conductivity of composite material；Porous structure may advantageously facilitate ion and quickly transmit and expand in electrode interior
It dissipates, to improve the high rate performance and cyclical stability of electrode material.
The present invention uses egg white for carbon source, is made porousT-Nb2O5/ egg white carbon composite.Egg white belongs to recyclable organism
Matter realizes egg white high-efficiency resource recycling.Preparation process is simply green, small to equipment corrosion, has environment friendly.Can have
Effect improves lithium ion super capacitor performance, reduces electrode material production cost.
(1) preparation process and products thereof characterizes
Embodiment:
1) egg white pre-processes: yolk being removed egg white retained, after mixing evenly for use.
2) 0.2 g niobic acid ammonium oxalic acid salt hydrate (C4H4NNbO9·xH2O；99.99%) 10 mL deionized waters are added to
In, it is added to after stirring in 60 mL egg white, continues 30 min of agitating solution to milky white after 0.5 mL, 2 mol/L HCl is added dropwise
Color, mixed emulsion move into 100 ml hydrothermal reaction kettles.
3) reaction kettle is put into baking oven, 24 h of hydro-thermal reaction, naturally cools to room temperature at 180 DEG C, to brown precipitate
Object is filtered, is freeze-dried, and obtains mixture.
4) mixture is placed in crucible, moves into tube furnace under nitrogen atmosphere, is warming up to the heating rate of 2 DEG C/min
700 DEG C, 2 h of constant temperature obtains combination product.
5) multiple with deionized water and washes of absolute alcohol, it is ground after dry, obtains lithium ion super capacitor with porousT-Nb2O5/ egg white carbon electrode material.
It is above porousT-Nb2O5The SEM of/egg white carbon material schemes as shown in Figure 1, after hydro-thermal-annealing, composite material
Irregular loose spherical structure, nanosphere surfaces versus rough is presented.Fig. 2 is that the TEM of composite material schemes, therefrom can be clear
See that carbon ball has pore structure abundant.Fig. 3 is that the HRTEM of composite material schemes, and can significantly see Nb from Fig. 32O5Size
About 5 ~ 10 nm, and be evenly distributed in carbon ball, the Nb of this nano-scale2O5Lithium ion insertion/it is embedding go out during
It is capable of providing the lithium ion diffusion path of very-short-reach, to improve its surface fake capacitance chemical property.Nb2O5Nanoparticle
Spacing of lattice be 0.39 nm, correspond to orthorhombic phase Nb2O5(001) crystal face, illustrate to be successfully prepared porousT-Nb2O5/ egg
Clear carbon material.
Fig. 4 is the porous of embodiment preparationT-Nb2O5The XRD spectrum of/egg white carbon material.From fig. 4, it can be seen that the diffraction of sample
Peak corresponds toT-Nb2O5(001), (108), (181), (002), (380) and (182) diffraction crystal face (JCPDF:30-0873),
Explanation is successfully preparedT-Nb2O5/ egg white carbon material.
Fig. 5 is the porous of embodiment preparationT-Nb2O5The thermogravimetric analysis figure of/egg white carbon material and egg white carbon.As seen from Figure 5,
After temperature is raised to 800 DEG C,T-Nb2O5/ egg white carbon material final mass remnants are about 58.3%, and egg white carbonaceous amount remains
4.2% or so, to illustrateT-Nb2O5Nb in/egg white carbon material2O5Mass content be about 54%.
Fig. 6 is the porous of embodiment preparationT-Nb2O5The full spectrogram of the XPS of/egg white carbon material and egg white carbon.It will be appreciated from fig. 6 that
The XPS of composite material detects six apparent Nb 3d, C 1s, O 1s, Nb 3s, Nb 3p and N 1s characteristic peaks in composing entirely, card
Element group within the scope of bright sample near surface becomes Nb, C, N and O etc., and the presence of N, O element can effectively improve composite material
Capacitive property.
(2) application and its effect
It takes porous made from above-described embodimentT-Nb2O5/ egg white carbon electrode material is tested:
It willT-Nb2O5/ egg white carbon material, acetylene black (super P) and polyvinylidene fluoride (PVDF) press the quality of 80:10:10
Than being mixed in n-methyl-2-pyrrolidone (NMP) uniformly to form slurry, then slurry is uniformly coated on Cu foil, is made
Use pure metal lithium piece as to electrode and reference electrode, diaphragm selects porous polypropylene film (Celgard 2500), electrolyte
For the 1M LiPF6 for being dissolved in ethylene carbonate/dimethyl carbonate (EC/DMC, volume ratio 1:1) in the mixed solvent, it is assembled into
CR2032 type button cell carries out electrochemical property test.
Fig. 7 is the porous of embodiment preparationT-Nb2O5The cyclic voltammetry curve figure of/egg white carbon electrode material.As seen from Figure 7,
There is wide anode and cathode peak within the scope of 1.4 ~ 2.1 V in the cyclic voltammetry curve of institute's sample, this is because Nb2O5
The redox reaction and lithium ion of Rapid reversible are in Nb2O5Caused by quickly being transmitted in crystal.In addition, with sweep speed
Increase, the basic configuration of CV curve illustrates that electrode material has preferable invertibity there is no significantly deforming.
Fig. 8 is the porous of embodiment preparationT-Nb2O5The staircase chart of/egg white carbon electrode material capacitance.As seen from Figure 8, institute
Sample possesses reversible capacitance 168.8,153.7,144.0,127.6,115.4,100.3 and 87.2 mAh/g, corresponds respectively to
0.1, the 51.7% of electricity when electricity when 0.2,0.5,0.8,1,2 and 5 A/g, 5 A/g is 0.1 A/g, illustrate electrode have compared with
Good high rate performance.This may be to promote electronics quickly to transmit to improve electrode material due to the good electric conductivity of carbon skeleton
Utilization rate.
Fig. 9 is the constant current charge-discharge curve of the electrode material of embodiment preparation.As seen from Figure 9, the constant current charge-discharge of sample
Curve does not occur significantly deforming with the increase of current density, illustrates that electrode material has preferable capacitive property and multiplying power
Performance.
Figure 10 is the specific capacity of the electrode material of embodiment preparation with the variation diagram of cycle-index.As seen from Figure 10, implement
Example preparation electrode material it is more stable in cyclic process and circulation 1000 times after still have higher capacity retention, illustrate its tool
There is outstanding cyclical stability.
With porous made from embodimentT-Nb2O5The electrode slice that/egg white carbon electrode material is formed has outstanding capacitive character
Energy.When current density increases to 5 A/g from 0.1 A/g, electricity conservation rate reaches 51.7%, in the case where current density is 0.8 A/g
Constant current charge-discharge 1000 times, capacity retention ratio 88.1%.
Claims (8)
1.T-Nb2O5The preparation method of/egg white carbon composite, which is characterized in that niobic acid ammonium oxalic acid salt hydrate is added to water
In, it is added in egg white after stirring, continues agitating solution to milky after dilute hydrochloric acid is added dropwise, hydro-thermal reaction freezes dry after filtering
It is dry, it then anneals in nitrogen atmosphere, last cleaned, dry, grinding obtains the electrode material.
2. the method as described in claim 1, which is characterized in that in the ratio of 0.2g:10 mL by niobic acid ammonium oxalic acid salt hydrate
It is add to deionized water.
3. the method as described in claim 1, which is characterized in that niobic acid ammonium oxalic acid salt hydrate and the adding proportion of egg white are
0.2g:60 mL.
4. the method as described in claim 1, which is characterized in that continue to stir after dropwise addition 0.5 mL, 2 mol/L dilute hydrochloric acid molten
30 min of liquid is to milky.
5. the method as described in claim 1, which is characterized in that 20~24 h of hydro-thermal reaction at 180~200 DEG C.
6. the method as described in claim 1, which is characterized in that be warming up to 700~800 with the heating rate of 2~5 DEG C/min
DEG C, rear 2~4 h of constant temperature.
7. prepared by the method as described in claim 1-6 is anyT-Nb2O5/ egg white carbon composite.
8. prepared by the method as described in claim 1-6 is anyT-Nb2O5/ egg white carbon composite is as electrode active material
Application.
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| CN112382515A (en) * | 2020-11-09 | 2021-02-19 | 贵州大学 | Oxygen defect T-Nb2O5Preparation method and application |
| CN114583132A (en) * | 2022-03-14 | 2022-06-03 | 华中科技大学 | Fast-charging energy storage material and preparation method and application thereof |
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