CN106129329A - A kind of graphene-based used as negative electrode of Li-ion battery combination electrode and preparation method thereof - Google Patents
A kind of graphene-based used as negative electrode of Li-ion battery combination electrode and preparation method thereof Download PDFInfo
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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Abstract
The invention discloses a kind of graphene-based used as negative electrode of Li-ion battery combination electrode, it is to be composited by foam metal, Graphene and transistion metal compound, wherein, described foam metal is as the support frame of combination electrode, described graphene uniform is deposited on this support frame, and described transistion metal compound then uniform deposition is on Graphene.Present invention also offers the preparation method of this combination electrode.The present invention is reasonable in design, practical, compared with prior art, its volume and capacity ratio that can be effectively improved graphene-based lithium ion battery and cyclical stability, therefore, the present invention has the highest practical value and wide application prospect, realizes industrialization provide good thinking and method for filling graphene battery soon.
Description
Technical field
The present invention relates to a kind of combination electrode, particularly relate to a kind of graphene-based used as negative electrode of Li-ion battery compound electric
Pole and preparation method thereof.
Background technology
Graphene battery is to utilize lithium ion characteristic of rapid, high volume shuttle between graphenic surface and electrode to open
A kind of new forms of energy battery issued, this new battery can be compressed to short a few minutes in the charging interval of a few hours.Therefore, not
Fill after graphene battery realizes industrialization soon, it will bring the change of battery industry, thus also promote new-energy automobile industry
Innovation.
But, the lithium battery cycle life that Graphene does negative pole is very poor, and charge/discharge rates is fast, directly affects its promote and
Actual application, this is primarily due to high power capacity, high cycle life and electrode performance stability and tends not to take into account, and it is the most former
Cause is: 1) existing class graphene carrier mobility is low, and electrical conductivity is less than Graphene, and internal resistance is big；2) graphenic surface without
Under poroid state, the quick intercalation of lithium ion is restricted.
In order to solve problem above, have two kinds of thinkings at present: 1) prepare physics, chemical property is adjustable has specified defect
The single-layer graphene of structure；2) the structure design of novel graphite alkene battery electrode: by the directional guide of skeleton, it is achieved lithium ion
Quick, stable embedding and deintercalation, and improve its volume capacity.But, for the first thinking, owing to its technology is difficult
Degree is big, is the most also difficult to breakthrough progress.Therefore, how to study and design novel battery structure, reduce graphite
The requirement of alkene, becomes the emphasis studied into those skilled in the art's present stage.
Summary of the invention
It is an object of the invention to provide a kind of graphene-based used as negative electrode of Li-ion battery combination electrode and preparation method thereof,
There is the problem that battery cycle life is poor, charge/discharge rates is fast in the lithium battery mainly solving to use Graphene to do negative pole.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of graphene-based used as negative electrode of Li-ion battery combination electrode, by foam metal, Graphene and transition metal compound
Thing is composited, and wherein, described foam metal is deposited on this as the support frame of combination electrode, described graphene uniform
On support frame, described transistion metal compound then uniform deposition is on Graphene.
As preferably, described foam metal is any one in nickel foam, foam copper, monel nano wire, and
The thickness of this foam metal is 0.005～5mm.
Further, when described foam metal is monel nano wire, its particle diameter is 10～100nm, a length of 100～
1000nm。
As preferably, described transistion metal compound is lithium titanate, titanium dioxide, nickel cobalt hydroxide, nickel cobalt sulfur generation point
Any one in spar, and the granularity of this transistion metal compound is 5～100nm, and thickness is 30～800nm.
Further, when described transistion metal compound is nickel cobalt hydroxide, its molecular formula is NixCoy(OH)2(x+y),
And x:y=1:(0.5～2).
As preferably, described Graphene thickness is 0.34～1.5nm.
Based on above-mentioned combination electrode, present invention also offers its preparation method, comprise the following steps:
(1) will rinse well as the foam metal of combination electrode support frame with deionized water and ethanol respectively, be dried
Stand-by；
(2) on the foam metal surface cleaned up, utilize gas phase and liquid phase sedimentation in-situ deposition Graphene, then use
Deionized water and alcohol flushing are clean, dried for standby；
(3) sample surfaces in step (2) gained deposits transistion metal compound, then does with deionized water and ethanol purge
Only, after drying, graphene-based used as negative electrode of Li-ion battery combination electrode is obtained.
Further, described foam metal is monel nano wire, and its preparation technology comprises the following steps:
A () is deposited with the thick silver electrode of one layer of 20nm in porous alumina formwork one end, as the negative pole of electro-deposition；
B () measures the nickel sulfate solution of 20ml, 2mM and the copper sulfate solution of 20ml, 1mM, mix homogeneously respectively, make
Presoma for electro-deposition preparation synthesis monel nano wire；
C () employing three-electrode method is under conditions of DC voltage 1V, temperature are 25 DEG C, on porous alumina formwork in situ
Electro-deposition 5min, wherein, silver-plated Woelm Alumina as working electrode, the Pt sheet of 2cm × 2cm × 0.2mm as to electrode,
Saturated calomel electrode is as reference electrode；
D () is clean by step (c) gained sample clean with deionized water and ethanol respectively, being then soaked in mass ratio is
The phosphoric acid of 1: 1 and chromic acid mixed solution carry out ultrasonic cleaning, removes porous alumina formwork, obtain monel nano wire.
Yet further, in described step (2), when foam metal is monel nano wire, the deposition of Graphene
Cheng Wei: monel nano wire is placed in tube furnace, and in the argon gas atmosphere of 900 DEG C, it is passed through acetylene, and it is incubated 5min.
Compared with prior art, the method have the advantages that
(1) present invention is reasonable in design, preparation method science, which employs foam metal, Graphene and transition metal compound
The design of three-decker that thing is composited, in this design, due to: 1) as the foam metal of combination electrode support frame itself
There is high conductivity and carrier mobility, reduce combination electrode internal resistance, thus solve class graphene carrier mobility
Low problem；2) support frame is that the uniform deposition of Graphene provides support, from spatially ensureing to embed and the stablizing of deintercalation
Property；3) macroporous structure of support frame self is that lithium ion realizes quick intercalation and provides feasible path, solves graphite
The problem of alkene surface atresia；4) on Graphene, deposit transistion metal compound, the macropore in combination electrode can be made full use of
The white space formed, improves the capacity in unit volume.Therefore, the present invention is greatly improved graphene-based lithium ion battery
Volume capacity and cyclical stability, efficiently solve the problem that graphene battery cycle life is poor, charge/discharge rates is fast.
(2) method preparing monel nano wire that the present invention uses, preparation method is simple, simple operation, and it utilizes
Nickel sulfate and copper sulfate solution prepare presoma, and combine porous alumina formwork and three-electrode method electro-deposition in situ goes out ambrose alloy
Alloy nano-wire, carries out ultrasonic cleaning and oxide removal the most again so that the monel nano wire prepared is possessing
While high conductivity, it is also equipped with macrovoid space structure, thus the support rib that the present invention that fitted well is to be reached
Frame uniform deposition Graphene and the purpose of transistion metal compound, effectively optimize the property of graphene battery prepared by the present invention
Energy.
(3) cost performance of the present invention is high, and each design link complements each other, tight association, and therefore, its practicality is very strong,
Battery performance is stable, reliable.It can be said that the present invention has good practical value and wide market application foreground, for filling soon
Graphene battery realizes industrialization and provides good thinking and method.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, and the mode of the present invention includes but are not limited to following enforcement
Example.
The invention provides the combination electrode of a kind of graphene-based used as negative electrode of Li-ion battery, it uses three-layer composite structure
Design, respectively foam metal (or array of metal lines), Graphene and transistion metal compound, wherein, described foam gold
Belonging to the support frame as combination electrode, described graphene uniform is deposited on this support frame, described transition metal
Compound then uniform deposition is on Graphene.
In above-mentioned three kinds of materials, foam metal is any one in nickel foam, foam copper, monel nano wire, and
And thickness is 0.005～5mm；Transistion metal compound is lithium titanate, titanium dioxide, nickel cobalt hydroxide, nickel cobalt sulfur generation point crystalline substance
Any one in stone, and granularity is 5～100nm, and thickness is 30～800nm；Graphene thickness is then 0.34～1.5nm.
The preparation process of the present invention is as follows:
(1) will rinse well as the foam metal of combination electrode support frame with deionized water and ethanol respectively, be dried
Stand-by；
(2) on the foam metal surface cleaned up, utilize gas phase and liquid phase sedimentation in-situ deposition Graphene, then use
Deionized water and alcohol flushing are clean, dried for standby；
(3) sample surfaces in step (2) gained deposits transistion metal compound, then does with deionized water and ethanol purge
Only, after drying, combination electrode of the present invention is obtained.
Below with the technique effect of a case introduction present invention.
Selected foam metal is monel nano wire；Transistion metal compound is nickel cobalt hydroxide, its molecule
Formula is NixCoy(OH)2(x+y), and x:y=1:(0.5～2).
It is deposited with the thick silver electrode of one layer of 20nm in porous alumina formwork one end, as the negative pole of electro-deposition, then distinguishes
Measuring the 1mM copper sulfate solution of 20ml, 2mM nickel sulfate solution and 20ml, mix homogeneously, as electro-deposition preparation synthesis nickel
The presoma of copper alloy nano wire.
Then, three-electrode method original position electro-deposition on porous alumina formwork is used to prepare monel nano wire.Specifically
Way is: using silver-plated Woelm Alumina as working electrode, the Pt sheet of 2cm × 2cm × 0.2mm is as to electrode, saturated sweet
Mercury electrode is as reference electrode；Then DC voltage be 1V, under conditions of temperature is 25 DEG C, by presoma electro-deposition 5min,
The most again by clean to sample deionized water and the ethanol purge of gained, and it is soaked in (phosphorus in the mixed solution of phosphoric acid and chromic acid
The mass ratio of acid and chromic acid is 1: 1)；Finally, remove porous alumina formwork, i.e. obtain length and be about a diameter of 50nm, long
Degree is the nickel-cobalt alloy nano line of 20 μm.
After obtaining nickel-cobalt alloy nano line, it is placed in tube furnace, and in the argon gas atmosphere of 900 DEG C, is passed through acetylene guarantor
Temperature 5min, obtains the thick graphene layer of about 1nm.Then, prepare one layer of nickel cobalt hydroxide in the electro-deposition of products therefrom surface, its
Granularity is about 50nm, and thickness is about 500nm.Finally, by clean to sample deionized water and the ethanol purge of gained, and in 60 DEG C
Under conditions of be vacuum dried 10h, obtain combination electrode.
In the glove box of argon atmospher, with lithium paper tinsel as negative pole, the combination electrode prepared of said method as positive pole, polypropylene many
Pore membrane be barrier film, the mixed solution of 1M LiPF6 be that electrolyte is assembled into button cell.Test the reversible capacity of this combination electrode
And charge-discharge performance.Test result surface: combination electrode prepared by this example, under the high rate charge-discharge of 2C, is put first
Electricity specific capacity reaches about 4508mAh/L；After 100 circulate, capacity maintenance dose is still 3824mAh/L；Coulombic efficiency is about
100%.
Change the preparation condition of combination electrode, its battery performance (composition of each layer of different composite electrode and the mensuration of thickness
Result) as shown in table 1.
Table 1
As it can be seen from table 1 change composition and thickness, the thickness of graphene layer, the transistion metal compound of framework metal
The thickness of layer and granularity, the specific capacity of meeting combination electrode prepared by appreciable impact and cyclical stability.Foam metal among these
As thickness for graphene layer of the support frame of combination electrode, its thickness and electrical conductivity, the carrier concentration of combination electrode
It is respectively provided with important function；And the thickness of graphene layer has a major impact for specific capacity and the electrical conductivity of system；Transition metal
Can compound kind and thickness granularity thereof, make full use of space, to promoting combination electrode volume and capacity ratio also important.
The present invention, by reasonable, the structure and handicraft design of science, has been greatly optimized the performance of graphene battery, has not only dropped
The low preparation requirement to Graphene, and the volume and capacity ratio of graphene-based lithium ion battery, battery cycle life and
Charge/discharge rates aspect there has also been the lifting of matter.Therefore, the present invention compared to existing technology for, technological progress is fairly obvious, its
There is prominent substantive distinguishing features and significantly progress.
Above-described embodiment is only one of the preferred embodiment of the present invention, should not be taken to limit the protection model of the present invention
Enclosing, all body design thought in the present invention and the change having no essential meaning made mentally or polishing, it is solved
Technical problem is the most consistent with the present invention, within all should being included in protection scope of the present invention.
Claims (9)
1. a graphene-based used as negative electrode of Li-ion battery combination electrode, it is characterised in that by foam metal, Graphene and transition
Metallic compound is composited, and wherein, described foam metal is as the support frame of combination electrode, described graphene uniform
Being deposited on this support frame, described transistion metal compound then uniform deposition is on Graphene.
One the most according to claim 1 graphene-based used as negative electrode of Li-ion battery combination electrode, it is characterised in that described
Foam metal is any one in nickel foam, foam copper, monel nano wire, and the thickness of this foam metal is
0.005～5mm.
One the most according to claim 2 graphene-based used as negative electrode of Li-ion battery combination electrode, it is characterised in that described
When foam metal is monel nano wire, its particle diameter is 10～100nm, a length of 100～1000nm.
4., according to the one graphene-based used as negative electrode of Li-ion battery combination electrode described in claims 1 to 3 any one, it is special
Levying and be, described transistion metal compound is that lithium titanate, titanium dioxide, nickel cobalt hydroxide, nickel cobalt sulfur are for appointing in spinelle
Meaning is a kind of, and the granularity of this transistion metal compound is 5～100nm, and thickness is 30～800nm.
One the most according to claim 4 graphene-based used as negative electrode of Li-ion battery combination electrode, it is characterised in that described
When transistion metal compound is nickel cobalt hydroxide, its molecular formula is NixCoy(OH)2(x+y), and x:y=1:(0.5～2).
6., according to the one graphene-based used as negative electrode of Li-ion battery combination electrode described in claim 1,2,3 or 5, its feature exists
In, described Graphene thickness is 0.34～1.5nm.
7. the preparation method of the combination electrode described in claim 1～6 any one, it is characterised in that comprise the following steps:
(1) will rinse well as the foam metal of combination electrode support frame with deionized water and ethanol respectively, dried for standby；
(2) on the foam metal surface cleaned up, utilize gas phase and liquid phase sedimentation in-situ deposition Graphene, then spend from
Sub-water and alcohol flushing are clean, dried for standby；
(3) sample surfaces in step (2) gained deposits transistion metal compound, cleaner with deionized water and ethanol purge,
After drying, graphene-based used as negative electrode of Li-ion battery combination electrode is obtained.
The preparation method of combination electrode the most according to claim 7, it is characterised in that described foam metal is monel
Nano wire, its preparation technology comprises the following steps:
A () is deposited with the thick silver electrode of one layer of 20nm in porous alumina formwork one end, as the negative pole of electro-deposition；
B () measures the nickel sulfate solution of 20ml, 2mM and the copper sulfate solution of 20ml, 1mM respectively, mix homogeneously, as electricity
The presoma of deposition preparation synthesis monel nano wire；
C () uses three-electrode method under conditions of DC voltage 1V, temperature are 25 DEG C, on porous alumina formwork, electricity is heavy in situ
Long-pending 5min, wherein, silver-plated Woelm Alumina is as working electrode, and the Pt sheet of 2cm × 2cm × 0.2mm is as to electrode, saturated
Calomel electrode is as reference electrode；
D () is clean by step (c) gained sample clean with deionized water and ethanol respectively, being then soaked in mass ratio is 1: 1
Phosphoric acid and chromic acid mixed solution in carry out ultrasonic cleaning, remove porous alumina formwork, obtain monel nano wire.
The preparation method of combination electrode the most according to claim 8, it is characterised in that in described step (2), when foam gold
When belonging to for monel nano wire, the deposition process of Graphene is: be placed in tube furnace by monel nano wire, and in 900
DEG C argon gas atmosphere in be passed through acetylene, and be incubated 5min.
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