CN104577052A - Electrochemical preparation method of polypyrrole/carbon fiber composite material electrode and application of polypyrrole/carbon fiber composite material electrode as positive electrode of lithium-ion battery - Google Patents
Electrochemical preparation method of polypyrrole/carbon fiber composite material electrode and application of polypyrrole/carbon fiber composite material electrode as positive electrode of lithium-ion battery Download PDFInfo
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Abstract
The invention discloses a preparation method of a polypyrrole/carbon fiber composite material electrode. A polypyrrole/carbon fiber composite material electrode (PPy-S-CF) is prepared by an in-situ polymerization method; and a polypyrrole/carbon fiber composite electrode (PPy-D-CF) is prepared by a steel mesh coating method, so that the positive electrode of the lithium-ion battery can be prepared in a one step. Compared with an existing preparation method of the positive electrode of the lithium-ion battery, the operation is relatively simple, convenient and fast; and the PPy-S-CF electrode and the PPy-D-CF electrode disclosed by the invention have relatively high specific discharge capacity, and relatively stable cycle performance.
Description
Technical field
The invention belongs to technical field of lithium ion, particularly relate to the electrochemical preparation method of polypyrrole/carbon fibre composite electrode and the application as lithium ion cell positive thereof, and by its obtained lithium ion battery.
Background technology
Along with the develop rapidly of global economy, facing mankind the problem in many evolutions, wherein the energy basis of depending on for existence as the mankind, is also the driving source of world economic growth, and thus energy problem also just becomes the much-talked-about topic discussed in 21 century world wide.Electric energy is due to clean, safety and the features such as facility demonstrate its superiority, and the develop rapidly of portable electric appts then forces chemical power source towards light-duty, small-sized, long life type development.This has also expedited the emergence of has high-energy-density, dexterous light, lithium ion battery industry that service life cycle is long.
Traditional anode material for lithium-ion batteries mainly adopts transition metal oxide, as the oxide etc. of cobalt-lithium oxide, nickel oxide lithium, manganese oxide lithium and vanadium.These materials, mainly based on noble metal, often have the defects such as mineral resources are limited, price is high, contaminated environment, preparation cost are high.Therefore, in order to the sustainable development of human society, research and development novel high-performance electrochemical power source and material just become particularly crucial.
Conducting polymer causes the extensive concern of people due to himself good conductivity and electro-chemical activity.In recent years, along with the progress of conductive polymer molecules design and fabrication technology, conducting polymer is applied to as positive electrode the great interest that field of lithium ion battery causes people.Wherein, polypyrrole is the conducting polymer finding comparatively early also to have passed through a large amount of system research.Polypyrrole, except having the common feature of other fragrant heterocyclic conducting polymer, also has that conductivity is high concurrently, good stability, electrochemical reversibility is strong, be easy to the features such as preparation and doping.These advantages are all that other numerous conducting polymer is incomparable.As far back as 1973, the people such as Gardini just synthesized the electric polypyrrole of black powder state, started the research that it can be used as anode material of lithium battery.But polypyrrole actual specific capacity is lower and have certain self discharge and limit its application in lithium battery.
Polypyrrole usually can by chemical oxidization method and electrochemical polymerization method preparation, and the more chemical oxidization method that utilizes prepares polypyrrole for anode material for lithium-ion batteries usually, and the follow-up like this multiple working procedure that needs could obtain lithium ion battery.And electrochemical polymerization method by the pyrrole monomer in electrolyte be polymerized on metal anode can obtain more complete, adhesion is strong and the good polypyrrole of chemical property, the poly-metal anode having gone up polypyrrole can directly as lithium ion cell positive application, and this method has the advantages such as simple to operate, quick.
Summary of the invention
The object of this invention is to provide polypyrrole/carbon fibre composite electrode and preparation method thereof.The present invention is under three electrode assemblies, adopt electrochemical polymerization, utilize situ aggregation method to prepare polypyrrole/carbon fibre composite electrode (PPy-S-CF) respectively and utilize steel mesh cladding process to prepare polypyrrole/carbon fiber combination electrode (PPy-D-CF).
Second object of the present invention is to provide the application as lithium ion cell positive of polypyrrole/carbon fibre composite electrode prepared by described situ aggregation method and polypyrrole/carbon fiber combination electrode prepared by steel mesh cladding process, the specific discharge capacity of raising battery that can be very large.
3rd object of the present invention is to provide polypyrrole/carbon fibre composite electrode prepared by polypyrrole/carbon fibre composite electrode of being prepared by described situ aggregation method and steel mesh cladding process as the obtained lithium ion battery of positive pole, and this lithium ion battery has higher specific discharge capacity and good cycle performance.
Below technical scheme of the present invention is illustrated.
A preparation method for polypyrrole/carbon fibre composite electrode, said method comprising the steps of:
(1) by Lithium perchlorate anhydrous (LiClO
4) join in acetonitrile (ACN) solvent, preparation lithium perchlorate concentration 0.1molL
-1liClO
4/ ACN blank solution, adds 0.1molL by pyrroles (Py)
-1liClO
4in/ACN blank solution, preparation obtains the electrolyte containing pyrroles, and described containing in the electrolyte of pyrroles, the concentration of pyrroles is 0.1molL
-1; Then add in the electrolyte containing pyrroles by carbon fiber (CF), be ultrasonicly fully mixed to get suspension electrolysis liquid, the carbon fiber contained in described suspension electrolysis liquid and the mass ratio of pyrroles are 1.5 ~ 2:1, preferred 1.8:1;
(2) three-electrode system is adopted, be for reference electrode to electrode, Ag/AgCl electrode with Pt sheet, the conductive substrates of insulating tape is pasted with for work electrode with one side, the suspension electrolysis liquid prepared with step (1) is for electrolyte, carry out cyclic voltammetry polymerization reaction, reaction terminates rear taking-up work electrode, with acetonitrile cleaning, tears insulating tape off, vacuumize, obtained polypyrrole/carbon fibre composite electrode.
In described step (2), the condition of described cyclic voltammetry polymerization reaction is: scanning voltage scope is-0.4 V ~ 1.3 V, and sweep speed is 10-100mV/s, and scanning hop count is 10-40 section.
In described step (2), described conductive substrates can be steel mesh or aluminium foil.
The present invention also provides the polypyrrole/carbon fibre composite electrode prepared by the preparation method of polypyrrole/carbon fibre composite electrode.Referred to as PPy-S-CF electrode in the present invention.
Described polypyrrole/carbon fibre composite electrode can directly be applied as lithium ion cell positive.
The present invention also provides the lithium ion battery obtained as positive pole by described polypyrrole/carbon fibre composite electrode.
The present invention also provides the preparation method of a kind of polypyrrole/carbon fiber combination electrode, said method comprising the steps of:
A () is by Lithium perchlorate anhydrous (LiClO
4) join in acetonitrile (ACN) solvent, preparation lithium perchlorate concentration 0.1molL
-1liClO
4/ ACN blank solution, adds 0.1molL by pyrroles (Py)
-1liClO
4in/ACN blank solution, preparation obtains the electrolyte containing pyrroles, and described containing in the electrolyte of pyrroles, the concentration of pyrroles is 0.1molL
-1;
(b) by carbon fiber (CF) and Kynoar (PVDF) in mass ratio 2:1 mix, add 1-METHYLPYRROLIDONE, carbon fiber slurry is made in stirring, carbon fiber slurry is coated in the one side of conductive substrates, the one side of the uncoated slurry of described conductive substrates is pasted with insulating tape, conductive substrates vacuumize after coating slurry, the conductive substrates of obtained coated carbon fibers;
C () adopts three-electrode system, be for reference electrode to electrode, Ag/AgCl electrode with Pt sheet, with the conductive substrates of coated carbon fibers for work electrode, the electrolyte containing pyrroles prepared with step (a) is for electrolyte, carry out cyclic voltammetry polymerization reaction, reaction terminates rear taking-up work electrode, with acetonitrile cleaning, tears insulating tape off, vacuumize, obtained polypyrrole/carbon fiber combination electrode.
In described step (b), the volumetric usage of 1-METHYLPYRROLIDONE generally counts 20 ~ 50mL/g with the quality of carbon fiber, preferably 30 ~ 40mL/g.
In described step (b), in conductive substrates, the coated weight of carbon fiber calculates by the conductive substrates of the coated carbon fibers weightening finish compared with the conductive substrates before coating obtained after vacuumize, i.e. carbon fiber coated weight=(the conductive substrates weight before the conductive substrates weight-coating of coated carbon fibers) × 2/3.
The Horizontal density variation of general control carbon fiber coated weight is 1 ~ 50mg/cm
2.
In described step (c), the condition of described cyclic voltammetry polymerization reaction is: scanning voltage scope is-0.4V ~ 1.3V, and sweep speed is 10-100mV/s, and scanning hop count is 10-40 section.
In described step (b), described conductive substrates can be steel mesh or aluminium foil.
The present invention also provides the polypyrrole/carbon fiber combination electrode prepared by the preparation method of polypyrrole/carbon fiber combination electrode.Referred to as PPy-D-CF electrode in the present invention.
Described polypyrrole/carbon fiber combination electrode can directly be applied as lithium ion cell positive.
The present invention also provides the lithium ion battery obtained as positive pole by described polypyrrole/carbon fiber combination electrode.
In two kinds of preparation methods provided by the invention, the size of described conductive substrates can adjust according to the dimensions size of positive pole needed for lithium ion battery to be prepared.
The one side that described insulating tape is attached to conductive substrates all carries out polymerization reaction to prevent the two-sided of conductive substrates.The size of insulating tape should be greater than the size of conductive substrates.
Conductive substrates for the preparation of lithium ion battery is generally sheet, strip, banded flat structure, so only need consideration two planar sections.
The present invention pyrroles used is used in electrochemical reaction, is ensure purity, use last as need through second distillation purifying.
Compared with prior art, advantage of the present invention is:
(1) the present invention is by having carried out compound by polypyrrole and carbon fiber, adds the conductivity of polymer; And introduce after carbon fiber carries out electrochemical polymerization, provide different polymerization environment, reduce the particle size of polypyrrole, add the contact area of polypyrrole and electrolyte, thus improve the utilance of active material, and then reach the object improving lithium ion battery specific discharge capacity.
(2) the present invention by utilizing electrochemical polymerization one step to obtain lithium ion cell positive on steel mesh, compares existing lithium ion cell positive manufacture method, operate easier, quick.
PPy-S-CF electrode provided by the invention is compared PPy electrode with PPy-D-CF electrode as lithium ion cell positive and is had higher specific discharge capacity, particularly PPy-D-CF electrode shows excellent performance as the positive pole of lithium ion battery, there is good conductivity, higher specific discharge capacity, comparatively stable cycle performance, therefore can be applied in lithium ion battery as the very potential positive pole of one.Meanwhile, electrochemical polymerization method one step provided by the invention obtains lithium ion cell positive, compares existing lithium ion cell positive manufacture method, has advantages such as reducing operating procedure.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of Platinum (PPy), in Fig. 1, and a figure amplification 1000 times, b figure amplification 6000 times, c figure amplification 25000 times.
Fig. 2 is the stereoscan photograph of polypyrrole/carbon fibre composite electrode (PPy-S-CF) prepared by situ aggregation method, in Fig. 2, and a figure amplification 400 times, b figure amplification 1000 times, c figure amplification 20000 times.Fig. 3 is the stereoscan photograph of polypyrrole/carbon fiber combination electrode (PPy-D-CF) prepared by steel mesh cladding process, in Fig. 3, and a figure amplification 5000 times, b figure amplification 15000 times, c figure amplification 80000 times.
The first charge-discharge curve chart of the lithium ion battery that Fig. 4 is PPy electrode, PPy-S-CF electrode, PPy-D-CF electrode are prepared as lithium ion cell positive.
The cycle performance figure of the lithium ion battery that Fig. 5 is PPy electrode, PPy-S-CF electrode, PPy-D-CF electrode are prepared as lithium ion cell positive.
Embodiment
Further illustrate technical scheme of the present invention by the following examples, but protection scope of the present invention is not limited thereto.
Embodiment 1:PPy electrode, PPy-S-CF electrode, PPy-D-CF electrode
Preparatory work of experiment: take 5.3200g Lithium perchlorate anhydrous (LiClO
4) join in acetonitrile (ACN) solution, preparation 500ml 0.1molL
-1liClO
4/ ACN blank solution, after mixing, is statically placed in shady and cool place stand-by.Produce by manual method of striking sheet the steel mesh disk that diameter is 12mm, disk uses absolute ethyl alcohol and acetone ultrasonic cleaning 10min successively, is then placed in air dry oven and dries, and after cooling, numbering is weighed.The required electrolyte of experiment needs now with the current, takes the pyrroles 0.3355g crossed through second distillation and pours 50mL0.1molL into
-1liClO
4in/ACN blank solution, after mixing and stirring, obtain 50ml pyrrole concentrations 0.1molL
-1liClO
4/ Py/ACN electrolyte.
Cut about 2cm × 2cm insulating tape, be pasted onto the one side of steel mesh disk, prevent polypyrrole at steel mesh double-sided polymerization.
The preparation of PPy electrode: by 50ml 0.1molL
-1liClO
4/ Py/ACN electrolyte is poured in three electrodes, with the steel mesh disk that one side is stained with insulating cement be work electrode, Pt sheet is for carrying out cyclic voltammetry polymerization to electrode, Ag/AgCl electrode for reference electrode on electrochemical workstation, scanning voltage scope is-0.4V ~ 1.3V, sweep speed is 50mV/s, and scanning hop count is 20 sections.Polymerization terminates rear acetonitrile cleaning electrode repeatedly, insulating tape of tearing, vacuumize 24h at being placed in 60 DEG C, obtained PPy electrode.
The preparation of PPy-S-CF electrode: take 0.6g carbon fiber (CF) and join 50ml 0.1molL
-1liClO
4in/Py/ACN electrolyte, ultrasonic 20min makes it be thoroughly mixed to form suspension, solution is poured in three electrodes, with the steel mesh disk that one side is stained with insulating cement be work electrode, Pt sheet is for carrying out cyclic voltammetry polymerization to electrode, Ag/AgCl electrode for reference electrode on electrochemical workstation, scanning voltage scope is-0.4V ~ 1.3V, sweep speed is 50mV/s, and scanning hop count is 20 sections.Polymerization terminates rear acetonitrile cleaning electrode slice repeatedly, insulating cement of tearing, vacuumize 24h at being placed in 60 DEG C, and obtained polypyrrole/carbon fibre composite electrode, is designated as PPy-S-CF electrode.
The preparation of PPy-D-CF electrode: the ratio being 2:1 in mass ratio by 0.08g carbon fiber (CF) and 0.04g Kynoar (PVDF) mixes, drip 3mL 1-METHYLPYRROLIDONE, stir and form slurry, coated weight is in the one side of the steel mesh disk of diameter 12mm, the uncoated slurry of steel mesh disk one side be pasted with insulating tape, 60 DEG C of vacuumize 24h, obtain former of the steel mesh of coated carbon fibers.Weigh after drying, weightening finish 3mg, namely carbon fiber coated weight is 2mg.In three electrodes, with 0.1molL
-1liClO
4/ Py/ACN solution is electrolyte, former of the steel mesh of coated carbon fibers is work electrode, Pt sheet is for being reference electrode to electrode, Ag/AgCl electrode, electrochemical workstation carries out cyclic voltammetry polymerization, scanning voltage scope is-0.4V ~ 1.3V, sweep speed is 50mV/s, and scanning hop count is 20 sections.Polymerization terminates rear acetonitrile cleaning electrode repeatedly, insulating tape of tearing, vacuumize 24h at being placed in 60 DEG C, and obtained polypyrrole/carbon fiber combination electrode, is designated as PPy-D-CF electrode.
Embodiment 2:
Respectively using the obtained PPy electrode of embodiment 1, PPy-S-CF electrode, PPy-D-CF electrode as the positive pole of lithium ion battery, take metal lithium sheet as negative pole, 1mol/L LiPF
6eC/DMC (V/V, 1:1) is electrolyte, and PP film is barrier film, in the glove box being full of argon gas, assemble button cell.
Carrying out electrochemical property test to the battery prepared, is under the charge-discharge velocity of 20mA/g in current density, 1mol/LLiPF
6eC/DMC (V/V, 1:1) in electrolyte, discharge and recharge and cycle performance test is carried out in 2.5V-4.2V voltage range, first charge-discharge curve chart as shown in Figure 4, cycle performance figure as shown in Figure 5, the result of Fig. 4-Fig. 5 is visible, and the first discharge specific capacity that PPy electrode, PPy-S-CF electrode, PPy-D-CF electrode make lithium ion cell positive is respectively 1.5mAhg
-1, 25.4mAhg
-1, 52.3mAhg
-1.PPy electrode, PPy-S-CF electrode, PPy-D-CF electrode are made specific discharge capacity after lithium ion cell positive circulates for 50 times and are respectively 3.1mAhg
-1, 15.4mAhg
-1and 42.6mAhg
-1.
Above result shows, polypyrrole of the present invention/carbon fibre composite electrode (PPy-S-CF electrode and PPy-D-CF electrode) is compared PPy electrode as lithium ion cell positive and is had higher specific discharge capacity, particularly PPy-D-CF electrode shows excellent performance as the positive pole of lithium ion battery, there is good conductivity, higher specific discharge capacity, comparatively stable cycle performance, therefore can be applied in lithium ion battery as the very potential positive pole of one.Meanwhile, electrochemical polymerization method one step provided by the invention obtains lithium ion cell positive, compares existing lithium ion cell positive manufacture method, has advantages such as reducing operating procedure.
Claims (10)
1. a preparation method for polypyrrole/carbon fibre composite electrode, is characterized in that said method comprising the steps of:
(1) Lithium perchlorate anhydrous is joined in acetonitrile solvent, preparation lithium perchlorate concentration 0.1molL
-1lithium perchlorate/acetonitrile blank solution, pyrroles is added 0.1molL
-1lithium perchlorate/acetonitrile blank solution in, preparation obtains the electrolyte containing pyrroles, and described containing in the electrolyte of pyrroles, the concentration of pyrroles is 0.1molL
-1; Then added by carbon fiber in the electrolyte containing pyrroles, be ultrasonicly fully mixed to get suspension electrolysis liquid, the carbon fiber contained in described suspension electrolysis liquid and the mass ratio of pyrroles are 1.5 ~ 2:1;
(2) three-electrode system is adopted, be for reference electrode to electrode, Ag/AgCl electrode with Pt sheet, the conductive substrates of insulating tape is pasted with for work electrode with one side, the suspension electrolysis liquid prepared with step (1) is for electrolyte, carry out cyclic voltammetry polymerization reaction, reaction terminates rear taking-up work electrode, with acetonitrile cleaning, tears insulating tape off, vacuumize, obtained polypyrrole/carbon fibre composite electrode.
2. the method for claim 1, is characterized in that, in described step (2), the condition of described cyclic voltammetry polymerization reaction is: scanning voltage scope is-0.4V ~ 1.3V, and sweep speed is 10-100mV/s, and scanning hop count is 10-40 section.
3. polypyrrole/carbon fibre composite electrode of preparing of method as claimed in claim 1 or 2.
4. polypyrrole/carbon fibre composite electrode as claimed in claim 3 is as the application of lithium ion cell positive.
5. polypyrrole/carbon fibre composite electrode as claimed in claim 3 is as the obtained lithium ion battery of lithium ion cell positive.
6. a preparation method for polypyrrole/carbon fiber combination electrode, is characterized in that said method comprising the steps of:
A Lithium perchlorate anhydrous joins in acetonitrile solvent by (), preparation lithium perchlorate concentration 0.1molL
-1lithium perchlorate/acetonitrile blank solution, pyrroles is added 0.1molL
-1lithium perchlorate/acetonitrile blank solution in, preparation obtains the electrolyte containing pyrroles, and described containing in the electrolyte of pyrroles, the concentration of pyrroles is 0.1molL
-1;
(b) by carbon fiber and Kynoar in mass ratio 2:1 mix, add 1-METHYLPYRROLIDONE, carbon fiber slurry is made in stirring, carbon fiber slurry is coated in the one side of conductive substrates, the one side of the uncoated slurry of described conductive substrates is pasted with insulating tape, conductive substrates vacuumize after coating slurry, the conductive substrates of obtained coated carbon fibers;
C () adopts three-electrode system, be for reference electrode to electrode, Ag/AgCl electrode with Pt sheet, with the conductive substrates of coated carbon fibers for work electrode, the electrolyte containing pyrroles prepared with step (a) is for electrolyte, carry out cyclic voltammetry polymerization reaction, reaction terminates rear taking-up work electrode, with acetonitrile cleaning, tears insulating tape off, vacuumize, obtained polypyrrole/carbon fiber combination electrode.
7. method as claimed in claim 6, it is characterized in that in described step (c), the condition of described cyclic voltammetry polymerization reaction is: scanning voltage scope is-0.4V ~ 1.3V, and sweep speed is 10-100mV/s, and scanning hop count is 10-40 section.
8. polypyrrole/carbon fiber combination electrode of preparing of method as claimed in claims 6 or 7.
9. polypyrrole/carbon fiber combination electrode as claimed in claim 8 is as the application of lithium ion cell positive.
10. polypyrrole/carbon fiber combination electrode as claimed in claim 8 is as the obtained lithium ion battery of lithium ion cell positive.
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| CN109768224A (en) * | 2019-01-11 | 2019-05-17 | 五邑大学 | A kind of preparation method based on growth in situ copper oxide/cobalt acid nickel nanowire composite negative electrode of lithium ion battery |
| CN109768224B (en) * | 2019-01-11 | 2021-09-03 | 五邑大学 | Preparation method of lithium ion battery cathode based on in-situ growth of copper oxide/nickel cobaltate nanowire composite material |
| CN110518207A (en) * | 2019-08-23 | 2019-11-29 | 中国工程物理研究院化工材料研究所 | A kind of flexibility ammonium ion full battery and preparation method thereof |
| CN113690057A (en) * | 2021-08-24 | 2021-11-23 | 湖南大学 | Phytic acid electrochemical oxidation-polypyrrole/carbon fiber composite material and preparation method and application thereof |
| CN113690057B (en) * | 2021-08-24 | 2022-08-02 | 湖南大学 | Phytic acid electrochemical oxidation-polypyrrole/carbon fiber composite material and preparation method and application thereof |
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