CN106654232A - Preparation method of laminar composite for negative electrode of secondary metal lithium battery - Google Patents
Preparation method of laminar composite for negative electrode of secondary metal lithium battery Download PDFInfo
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- CN106654232A CN106654232A CN201710051717.2A CN201710051717A CN106654232A CN 106654232 A CN106654232 A CN 106654232A CN 201710051717 A CN201710051717 A CN 201710051717A CN 106654232 A CN106654232 A CN 106654232A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/043—Processes of manufacture in general involving compressing or compaction
- H01M4/0435—Rolling or calendering
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/381—Alkaline or alkaline earth metals elements
- H01M4/382—Lithium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method of a laminar composite for a negative electrode of a secondary metal lithium battery. The preparation method comprises the following steps: (1) taking a metal lithium sheet and a compound additive; uniformly distributing the compound additive on the surface of the metal lithium sheet; pressing the compound additive into the metal lithium sheet by adopting a rolling method; (2) folding a composite of the metal lithium sheet and the compound additive and rolling to obtain a laminar-structure additive-metal lithium composite sheet; (3) repeating the step (2) for a plurality of times to obtain the composite with different metal lithium layer thicknesses. According to the preparation method provided by the invention, operation can be carried out through conventional roller rolling equipment and the process has the characteristics of convenience for operation and simple process. By adopting the method provided by the invention, the laminar composite of a lithiated nano-material and a lithium sheet is obtained; when the laminar composite is used as the negative electrode of the secondary metal lithium battery, related problems of growth of lithium dendrites can be solved.
Description
Technical field
The invention belongs to secondary cell field, and in particular to a kind of preparation side of the electrode material of secondary metals lithium battery
Method.
Background technology
One of most widely used as the world today and most promising battery of lithium metal battery, with specific energy and
Discharge performance height, work and the high and lower-cost advantage of storage life length, safety operation performance.With Li-S batteries, Li- it is empty
The appearance of the novel high-capacity lithium battery such as pneumoelectric pond, the safety applications of Li metal negative electrodes become energy storage system of future generation
Decisive factor.
Li metals are considered always the optimal negative material of rechargeable lithium battery, and it has high theoretical specific capacity
(3860mAh g-1), low-density (0.59g cm-3) and most negative electrochemical potential (comparison with standard hydrogen electrode about -3.04V) etc.
Excellent properties.Yet with the no-load bulk properties of Li metal negative electrodes, its exist in recharge/discharge process dendritic growth and
Low coulombic efficiency (CE) problem, causes not yet to be commercialized so far based on the rechargeable battery of Li metal negative electrodes.
The method that at present conventional suppression Li dendrite is formed has：Stable SEI films are formed in situ, dystopy forms surface and applies
Layer, mechanical close, selfreparing electrostatic screen method etc..These methods each solve to a certain extent Li metal negative electrodes and are filling
The low problem of dendritic growth and coulombic efficiency during discharge cycles, but certain limiting factor is individually present.It is newest to grind
Study carefully progress to show, from the angle for building lithium combination electrode, stability of the Li metals in charge and discharge cycles can be effectively improved.
Rational design can change Li metal deposit preferences, fundamentally improve the low problem of dendritic growth and coulombic efficiency.However,
For majority of material, its between elemental lithium combine it is weak, i.e., with thin lithium.Therefore, a kind of pervasive composite square is developed
Application of the method to lithium metal battery negative pole is significant.
The content of the invention
For the weak point that this area is present, it is contemplated that proposing that a kind of secondary metals cathode of lithium battery stratiform is answered
The preparation method of compound.Nanometer powdery compound additive is combined with lithium metal simple substance by roll-to-roll method, is had
The additive of layer structure-lithium metal composite sheet.
It is another object of the present invention to propose that the preparation method has obtained lithium metal battery composite pole piece.
Third object of the present invention is to propose the lithium metal battery containing gained composite pole piece.
The technical scheme for realizing the object of the invention is：
A kind of preparation method of secondary metals cathode of lithium battery laminated composites, it includes step：
(1) metal lithium sheet and compound additive that thickness is 0.2～2mm are taken, compound additive is evenly distributed on into metal
The surface of lithium piece, and compound additive is pressed in metal lithium sheet using roll-in method；
Wherein, the compound additive is selected from metal nano powder, non pinetallic nano powder, lamellar structure compound, two wieners
Rice piece one kind of multiple；
(2) compound of compound additive and metal lithium sheet is folded, roll-in is carried out, the additive-gold of layer structure is obtained
Category lithium composite sheet；
(3) step (2) is repeated several times, the compound with different metal lithium layer thickness is obtained.
Wherein, one kind in the metal nano powder chosen from Fe, copper, nickel metal nano powder, the particle diameter of metal nano powder is little
In 300 nanometers；The one kind of layered structural compounds in hexagonal boron nitride, molybdenum bisuphide, tungsten disulfide.
Wherein, the one kind of the non pinetallic nano powder in silica flour, graphite powder, powdered carbon, the particle diameter of non pinetallic nano powder
For 50～1000 nanometers；The two-dimensional nano piece is selected from Graphene, graphene oxide, boron nitride nanosheet, molybdenum disulfide nano
Piece, tungsten disulfide nano slices, Ti3C2One kind in nanometer sheet, lamellar spacing is less than 50 nanometers.Nanometer used in the inventive method
Powder is solid phase powder, does not deposit reuniting effect in the liquid phase, and uniform paving is sprinkled upon lithium piece surface.
Wherein, described two-dimensional nano piece Ti3C2It is to peel off to obtain using following ultrasound：Under the conditions of gas shield, use
HF acid etches Ti3AlC2, to HF acid and Ti3AlC2Mixture it is ultrasonically treated, then cleaned again and freezed.
Wherein, carry out roll-in two are 0.02-1mm to the gap between roller.
Wherein, the compound additive for obtaining after each roll-in and the thickness of the compound of metal lithium sheet are the 1/2- before roll-in
1/10, the compound additive obtained after each roll-in and the compound area of metal lithium sheet for step (1) virgin metal lithium piece face
Long-pending 2～10 times；The number of times for being repetitively folded roll-in is 2～15 times.
Further, the mass ratio of the metal lithium sheet and compound additive is 9:1～1:Between 1.Finally it is combined
The thickness of the compound of additive and metal lithium sheet is 0.2～2mm.
The additive that preparation method of the present invention is prepared-lithium metal composite sheet.
Secondary metals lithium battery containing described additive-lithium metal composite sheet.
The beneficial effects of the present invention is：
Preparation method proposed by the present invention, can be operated with conventional to roller rolling equipment, and the technique has operation
Conveniently, the characteristics of process is simple.Using the method for the present invention, the nano material and lithium piece laminated composites of close lithiumation are obtained,
When the laminated composites are used as secondary metals cathode of lithium battery, the relevant issues of lithium dendrite growth can be improved, battery has more
Little overpotential and longer cycle life.
Description of the drawings
Fig. 1 is Ti in embodiment 1,2,33C2The preparation flow figure of-Li compounds.
Fig. 2 is laminate Ti of embodiment 13C2The section SEM photograph of-Li compounds.
Fig. 3 is laminate Ti of embodiment 13C2The XRD diffracting spectrums of-Li compounds.
Fig. 4 is Ti in embodiment 1,2 and comparative example3C2The cycle performance figure of-Li, G-Li and simple substance lithium piece Symmetrical cells.
Fig. 5 is Ti in embodiment 1,2 and comparative example3C2The high rate performance figure of-Li, G-Li and simple substance lithium piece Symmetrical cells.
Fig. 6 is Ti in embodiment 1 and comparative example3C2- Li, simple substance lithium piece is negative pole, and sulphur-carbon is the full battery of lithium sulphur of positive pole
Capacity versus cycle performance map.
Fig. 7 is Ti in embodiment 1 and comparative example3C2- Li, simple substance lithium piece is negative pole, and sulphur-carbon is the full battery of lithium sulphur of positive pole
High rate performance figure.
Fig. 8 is the section SEM photograph of the laminate Cu-Li compound of embodiment 3.
Fig. 9 is the cycle performance figure of the laminate Cu-Li Symmetrical cells of embodiment 3.
Specific embodiment
Detailed description below is used to illustrate the present invention, but should not be construed as limiting the invention.
In embodiment, if no special instructions, technological means used is this area conventional technique means.
Rolling equipment be the Hefei section crystalline substance electronic roll squeezers of MSK-MR100DC, to the gap between roller be 0.02-1mm, pressure
For 10MPa.
Embodiment 1：
Operating process such as Fig. 1,
A kind of Ti3C2- Li sheet-like composites, it is made by the steps and obtains：
Mass ratio is taken for 9:1 lithium piece and Ti3C2The thickness of nanometer sheet powder, wherein lithium piece is 1mm, and area is 4cm2,
Ti3C2The thickness of nanometer sheet is 5nm, by Ti3C2Nanometer sheet powder spoon paving spills the surface for being uniformly distributed in elemental lithium, level
Push gap for 0.5mm to roller in, to carry out roll-in make Ti3C2Nanometer sheet powder is entered in lithium metal, Ti after roll-in3C2- lithium is multiple
The area of compound is 2 times of original lithium piece area.
By the Ti3C2- Li composite sheets carry out doubling and roll-in again, keep Ti3C2The area of-Li is 4cm2.It is repetitively folded
With calandering steps 10 times, the final Ti for obtaining layer structure3C2- Li composite sheets, by composite sheet the electrode slice of diameter 6mm is stamped into.
Ti3C2Visible Fig. 1 of preparation process figure of-Li sheet-like composites.
Wherein, Ti3C2The preparation of nanometer sheet is obtained using ultrasound stripping：With HF acid etches Ti3AlC2, to HF acid and
Ti3AlC2Mixture it is ultrasonically treated, then cleaned again and freezed and obtained, Ti3C2Nanometer sheet lamellar spacing is 5 nanometers.
Ti3C2Each step of nanometer sheet preparation process is all in N2Protection under carry out avoiding Ti3C2Oxidation.
To gained Ti3C2Pattern and composition of-Li sheet-like composites etc. are characterized, as a result referring to shown in Fig. 2 and Fig. 3.From
Ti in Fig. 23C2The cross sectional image of-Li compounds is it is observed that the thickness in monolayer of the lithium metal of stratiform is about 10-50 microns.
XRD diffraction patterns can be seen that Ti from Fig. 33C2Successfully it is combined with lithium metal.
To gained Ti3C2- Li sheet-like composite electrode groups are circulated charge-discharge test, charge and discharge cycles into Symmetrical cells
The result of 200 times is shown in Fig. 4.Symmetrical cells test shows, compared with pure lithium electrode, Ti3C2- Li combination electrodes are in whole circulation
Show more stable voltage's distribiuting, lower overpotential, 1mA/cm2Initial overpotential 32mV under current density, 200 circulations
Afterwards overpotential only increases by 1.5%, and good high rate performance, 3mA/cm2Initial overpotential 106mV, 5mA/ under current density
cm2Initial overpotential 206mV (Fig. 4 and Fig. 5) under current density.
With Ti3C2- Li compounds are negative pole, with S-C as positive pole, with polyethylene as barrier film, with 1MLiTFSI/DOL+DME
(1:1) the full battery for electrolyte shows good chemical property (Fig. 6 and Fig. 7).The full battery is initially put under 1C electric currents
Capacitance is more than 900mAh g-1, capacity is maintained at 750mAh g after 200 circulations-1More than, the energy of the full battery of correspondence is close
Spend for 695Wh kg-1.200 coulombic efficiencies of circulation keep more than 90%.Additionally, the full battery also show it is good forthright again
Can, capacity is maintained at 400mAh g under 5C electric currents-1More than.
Embodiment 2
A kind of G-Li sheet-like composites (G represents Graphene), its preparation method with embodiment 1, except for the difference that will substantially
Ti3C2Nanometer sheet powder is replaced with graphene powder.The Graphene for wherein using is prepared by the method for peeling off blocky graphite by ultrasound
Obtain, graphene sheet layer thickness is 1nm.
The chemical property of gained G-Li sheet-like composites is characterized, as a result referring to Fig. 4 and Fig. 5.Symmetrical cells are surveyed
Take temperature bright, G-Li combination electrodes are in 1mA/cm2Charge and discharge cycles are carried out under current density, its overpotential to present first reduce and increase afterwards
Plus trend, its initial overpotential be 106mV, 200 circulation after overpotential increase by 114%.
Embodiment 3
A kind of Cu-Li sheet-like composites, its preparation method is substantially with embodiment 1.Except for the difference that by Ti3C2Nanometer sheet powder
It is that Cu nanometer powders replace with particle diameter, the particle diameter of Cu nanometer powders is 100～200nm.The number of repetition for folding roll-in is six times.
Pattern to gained Cu-Li sheet-like composites etc. is characterized, as a result referring to Fig. 8.With Ti3C2- Li is similar to, and is combined
Thing present it is laminar structured, but due to the number of repetition for folding roll-in it is different, corresponding lamellar spacing and Ti3C2- Li is different.
The chemical property of gained Cu-Li sheet-like composites is characterized.Fig. 9 is following for stratiform Cu-Li Symmetrical cells
Ring performance map.Symmetrical cells test shows, compared with pure lithium electrode, Cu-Li combination electrodes show more steady in whole circulation
Fixed voltage's distribiuting, in 1mA/cm2Initial overpotential is 55mV under current density.
Comparative example
With enter any additive without roll-in lithium piece as a comparison, the diameter and thickness of lithium piece is with embodiment 1.Use the lithium
Piece constitutes Symmetrical cells, uses 1mA/cm2Electric current be circulated charge-discharge test, as a result see Fig. 4 and Fig. 5.The mistake of first cycle
Current potential is 70mV, after 200 circulations overpotential more than 400mV, and in whole test process overpotential fluctuation greatly, stability
Difference.
With elemental lithium as negative pole, with S-C as positive pole, battery is helped in assembling, and the assembling of full battery is same as Example 1.Should
First discharge capacity is 900mAh g to full battery under 1C electric currents-1, capacity is only 430mAh g after 100 circulations-1.Times
Rate the performance test results show, under the discharging condition of 5C, battery capacity is less than 100mAh g-1。
Embodiment above is only that the specific embodiment to the present invention is described, and not the scope of the present invention is entered
Row is limited, and those skilled in the art can also do on the basis of existing technology numerous modifications and variations, set without departing from the present invention
On the premise of meter spirit, various modifications and improvement that this area ordinary skill technical staff makes to technical scheme,
All should fall in the protection domain of claims of the present invention determination.
Claims (9)
1. a kind of preparation method of secondary metals cathode of lithium battery laminated composites, it is characterised in that including step：
(1) it is 0.2～2mm metal lithium sheets and compound additive to take thickness, and compound additive is evenly distributed on into metal lithium sheet
Surface, and compound additive is pressed in metal lithium sheet using roll-in method；Wherein, the compound additive is selected from metal nano
Powder, non pinetallic nano powder, lamellar structure compound, two-dimensional nano piece one kind of multiple；
(2) compound of compound additive and metal lithium sheet is folded, roll-in is carried out, the additive-lithium metal of layer structure is obtained
Composite sheet；
(3) step (2) is repeated several times, the compound that lithium layer thickness in compound is 0.1～20 μm is obtained.
2. preparation method according to claim 1, it is characterised in that the metal nano powder chosen from Fe, copper, nickel metal are received
One kind in ground rice, the particle diameter of metal nano powder is less than 300 nanometers；Layered structural compounds selected from hexagonal boron nitride, two
One kind in molybdenum sulfide, tungsten disulfide.
3. preparation method according to claim 1, it is characterised in that the non pinetallic nano powder selected from silica flour, graphite powder,
One kind in powdered carbon, the particle diameter of non pinetallic nano powder is 50～1000 nanometers；The two-dimensional nano piece is selected from Graphene, oxidation stone
Black alkene, boron nitride nanosheet, molybdenum disulfide nano sheet, tungsten disulfide nano slices, Ti3C2One kind in nanometer sheet, lamellar spacing is little
In 20 nanometers.
4. preparation method according to claim 3, it is characterised in that two-dimensional nano piece Ti3C2It is to be surpassed using following
Sound is peeled off and obtained：Under the conditions of gas shield, with HF acid etches Ti3AlC2, to HF acid and Ti3AlC2Mixture it is ultrasonically treated,
Then cleaned again and freezed.
5. preparation method according to claim 1, it is characterised in that carry out roll-in two are to the gap between roller
0.02-1mm。
6. preparation method according to claim 1, it is characterised in that the compound additive for obtaining after roll-in every time and metal
The thickness of lithium piece compound be roll-in before composite thickness 1/2-1/10, compound additive and metal lithium sheet compound after roll-in
Area be changed into 2-10 times before roll-in；The number of times for being repetitively folded roll-in is 2～15 times.
7. the preparation method according to any one of claim 1～6, it is characterised in that the compound additive and lithium metal
The mass ratio of piece is 1:1～1:Between 9, the compound additive for finally obtaining and the thickness of metal lithium sheet compound is 0.2～
2mm。
8. additive-lithium metal composite sheet that preparation method described in any one of claim 1～7 is prepared.
9. containing the secondary metals lithium battery of the additive described in claim 8-lithium metal composite sheet.
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Cited By (17)
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| CN107799736A (en) * | 2017-09-22 | 2018-03-13 | 山东大学 | A kind of lithium metal composite negative pole of three-dimensional self-supporting parent lithium carrier encapsulation and preparation method thereof |
| CN108346800A (en) * | 2018-02-08 | 2018-07-31 | 北京航空航天大学 | A kind of cathode richness lithium additive improving lithium ion battery coulombic efficiency for the first time |
| CN108735984A (en) * | 2018-04-11 | 2018-11-02 | 燕山大学 | A kind of preparation method of molybdenum disulfide/carbonization titanium composite material |
| CN108923036A (en) * | 2018-07-17 | 2018-11-30 | 浙江大学山东工业技术研究院 | The preparation method of carbon-lithium composite powder and preparation method thereof, lithium metal electrode for secondary battery |
| CN109037626A (en) * | 2018-07-20 | 2018-12-18 | 浙江大学 | A kind of alkali metal base cathode and its preparation method and application |
| CN109576454A (en) * | 2018-12-19 | 2019-04-05 | 深圳先进技术研究院 | Preparation method, metal nano plate, purposes and the negative electrode active material of metal nano plate |
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| CN107799736A (en) * | 2017-09-22 | 2018-03-13 | 山东大学 | A kind of lithium metal composite negative pole of three-dimensional self-supporting parent lithium carrier encapsulation and preparation method thereof |
| JP7239591B2 (en) | 2018-01-09 | 2023-03-14 | サウジ アラビアン オイル カンパニー | Nanocomposite electrode materials for use in high temperature and high pressure rechargeable batteries |
| JP2021509761A (en) * | 2018-01-09 | 2021-04-01 | サウジ アラビアン オイル カンパニー | Nanocomposite electrode material for use in high temperature and high pressure rechargeable batteries |
| CN108346800A (en) * | 2018-02-08 | 2018-07-31 | 北京航空航天大学 | A kind of cathode richness lithium additive improving lithium ion battery coulombic efficiency for the first time |
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