CN109103456A - A kind of preparation method of the compound porous collector for lithium an- ode protection - Google Patents
A kind of preparation method of the compound porous collector for lithium an- ode protection Download PDFInfo
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- CN109103456A CN109103456A CN201810701013.XA CN201810701013A CN109103456A CN 109103456 A CN109103456 A CN 109103456A CN 201810701013 A CN201810701013 A CN 201810701013A CN 109103456 A CN109103456 A CN 109103456A
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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
- H01M4/64—Carriers or collectors
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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
- H01M4/64—Carriers or collectors
- H01M4/66—Selection of materials
- H01M4/661—Metal or alloys, e.g. alloy coatings
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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
A kind of preparation method of the compound porous collector for lithium an- ode protection, the preparation method include the following steps: that (1) weighs a certain proportion of copper powder, pore creating material, close lithium active material powder and uniformly mixes, obtain mixed-powder；(2) mixed-powder is taken, tabletting is carried out with mold, obtains thin layer disk, 1100-1500 DEG C of heat preservation calcination processing 1-4h is then warming up under protective atmosphere, obtains pre-composite porous current collector；(3) pre-composite porous current collector is soaked in the dilute hydrochloric acid of 5-15% to remove pore creating material, then removes remaining hydrochloric acid with deionized water again, drying process obtains compound porous collector.Preparation method raw material resources of the invention are abundant and constituent is controllable, on the one hand obtained compound porous collector provides huge receiving volume for lithium deposition, on the other hand lithium ion homogeneous nucleation can be induced, the growth of dendrite is prevented, to realize the higher coulombic efficiency of lithium ion battery and longer cycle life.
Description
(1) technical field
The invention belongs to field of lithium, are related to a kind of preparation of compound porous collector for lithium an- ode protection
Method.
(2) background technique
Lithium metal is a kind of very promising negative electrode material, its theoretical capacity is up to 3860mAh/g, is equivalent to biography
10 times of system graphite electrode capacity, if can be applied will greatly improve the energy density of existing lithium ion battery.In recent years,
Due to the high-energy density of lithium-sulfur cell and lithium sky battery, lithium anode is constantly subjected to the extensive concern of researcher,
So become the emphasis and hot spot of research.However, on the one hand lithium metal will form not because it can generate dendrite during removal lithium embedded
Stable SEI causes electrolyte and lithium metal continuously to consume, and reduces the efficiency and cycle life of battery；Another party
Face leads to internal short-circuit of battery since dendrite can pierce through diaphragm, make battery failure, more seriously may lead battery
Fire even explodes, and causes a series of safety issues.In order to inhibit the growth of Li dendrite, improving the security performance of lithium battery and follow
Ring service life, a large amount of researchers are dedicated to the correlative study of lithium anode protection.Up to the present, inhibit Li dendrite raw
Long, one of the effective ways of stable metal lithium, the collector for exactly constructing more functionalization replaces traditional plane copper collector,
This strategy can fundamentally induce the forming core of lithium to grow, and avoid the generation of Li dendrite, be the commercialization benefit of lithium an- ode
With bringing great hope.
(3) summary of the invention
Goal of the invention of the invention is to provide that a kind of raw material resources are abundant and constituent is controllable for lithium metal
On the one hand the preparation method of the compound porous collector of cathode protection, the compound porous collector provide huge appearance for lithium deposition
It receives volume, on the other hand can induce lithium ion homogeneous nucleation, prevent the growth of dendrite, to realize that lithium ion battery is higher
Coulombic efficiency and longer cycle life.
Technical solution of the present invention is specifically described below.
It is described compound the present invention provides a kind of preparation method of compound porous collector for lithium an- ode protection
Porous current collector includes the three-dimensional porous copper skeleton as main body and the close lithium active material that is supported on copper skeleton；It is prepared
Method includes the following steps:
(1) a certain proportion of copper powder, pore creating material, close lithium active material powder are weighed uniformly to mix, obtains mixed-powder；Institute
It states in mixed-powder, the mass content of pore creating material is 10-30wt%, and the mass content of close lithium active material is 10-20wt%, remaining
Amount is copper powder；
(2) mixed-powder that appropriate step (1) obtains is weighed, tabletting is carried out with mold, obtains thin layer disk, then protecting
It is warming up to 1100-1500 DEG C with the rate of 3-10 DEG C/min under shield atmosphere, calcination processing 1-4h is kept the temperature, obtains pre-composite porous collection
Fluid；
(3) to remove pore creating material, then again obtained pre-composite porous current collector is soaked in 5-15% dilute hydrochloric acid
Remaining hydrochloric acid is removed with deionized water, is placed in 50-80 DEG C of baking oven and is dried, compound porous afflux can be obtained
Body.
Step (1) of the present invention selects suitable pore creating material by the one or more close lithium active materials appropriate of addition, and
Pass through the good porous functionalization collector of the regulation preparation structure of ratio.
Further, the close lithium active material is Zn, Mg, Al, Si, ZnO, MgO, Al2O3Or SiO2One of or appoint
It anticipates several combinations.
Further, the pore creating material is calcium oxide, calcium carbonate or sodium carbonate；It is preferred that its purity is greater than 90%.It is described mixed
The content for closing pore creating material in powder is preferably 10-20wt%.
In step (2) of the present invention, for calcination temperature preferably at 1100-1400 DEG C, calcination time is preferably 2-4h.
In step (2) of the present invention, protective atmosphere is the group of one or both of argon gas, nitrogen arbitrary proportion when calcining
It closes, preferably its purity is greater than 90%.
Compared with current techniques, the beneficial effects are mainly reflected as follows:
(1) collector obtained designed by the present invention mainly has low lithium ion forming core mistake using close lithium active material
Current potential, to induce the uniform deposition of lithium ion during discharge.This new structure is able to achieve good chemical property,
On the one hand have benefited from the porous current collector being prepared with very large space, provide huge receiving volume for lithium deposition, separately
On the one hand the close lithium active material being dispersed on stephanoporate framework can reduce sedimentation potential, induce the expansion of lithium ion flux
It dissipates, makes lithium homogeneous nucleation, and then avoid the generation of dendrite, to realize high-performance (higher coulombic efficiency and longer circulation longevity
Life) lithium ion battery brings possibility.
(2) preparation method of the compound porous collector of the present invention is simple, and raw material resources are abundant, and constituent can
Control, can be adjusted according to actual needs.
(4) Detailed description of the invention
Fig. 1 be 1 composite powder of embodiment after mixing, be pressed into the digital photograph of disk.
Fig. 2 is that embodiment 1 suppresses obtained disk, the digital photograph after being sintered by high temperature.
Fig. 3 is SEM figure of the compound porous collector prepared by embodiment 1 under different enlargement ratios.
Fig. 4 is the chemical property that compound porous collector is assembled into button cell and blank sample prepared by embodiment 1
Figure, wherein current density is 2mA/cm2。
(5) specific implementation method
With specific embodiment, technical scheme is described further below, but protection scope of the present invention is unlimited
In this.
Embodiment 1
It takes 6g copper powders to be placed in mortar, 3g calcium carbonate is added, then adds 1g metallic aluminium powder, is sufficiently mixed, when grinding
Between about 1 hour.After completion to be ground.0.18g mixed-powder is weighed, is added in the mold that diameter is 12mm, utilizes tabletting
Machine is suppressed, pressure 20Mpa, and the retention time is 1 minute；Then the disk pressed high temperature process furnances are put into forge
Burn, under nitrogen atmosphere protection, be warming up at 1200 DEG C with the heating rate of 5 DEG C/min keep the temperature 2 hours and obtain it is pre-composite porous
Collector；The disk sintered is finally put into immersion 12 hours in 10% pre-configured dilute hydrochloric acid solution, finally again
It is rinsed with a large amount of deionized waters, it is ensured that remove remaining hydrochloric acid.It finally dries, can be obtained compound in 50 DEG C of convection oven
Porous current collector.
The porous current collector obtained by embodiment 1 carries out the assembling of button cell as follows.
With compound porous collector directly as electrode slice, electrolyte be 1M LiTFSI/DOL:DME (volume ratio 1:
1), wherein LiNO containing 0.1M3Additive, diaphragm be Celgard 2400, to electrode metal lithium sheet, using 2032 electrodes
The assembling of shell progress button cell.Check experiment using plane copper sheet as electrode, under identical capacity and current density into
Row test, wherein coulombic efficiency comparative diagram is shown in Fig. 4.In contrast, using compound porous collector prepared by the present invention identical
(2mA/cm under current density2), the unattenuated purpose of long circulating may be implemented, this mainly has benefited from this collector relative to flat
Face copper sheet has huge spatial volume, can accommodate more lithiums and allow lithium huge volume during removal lithium embedded swollen
It is swollen, it, can in addition importantly, evenly dispersed the small close lithium active material of forming core overpotential in three-dimensional framework of the invention
Lithium ion homogeneous nucleation is induced, the growth of dendrite is prevented, to realize higher coulombic efficiency and longer cycle life.
Embodiment 2
It takes 3g copper powders to be placed in mortar, 1.5g sodium carbonate is added, then add 0.5g Zinc oxide powder, is sufficiently mixed, grinds
Time consuming about 2 hours.It weighs 0.2g mixed-powder again later, is added in the mold that diameter is 12mm, is carried out using tablet press machine
Compacting, pressure 30Mpa, retention time are 5 minutes；Then the disk pressed is put into high temperature process furnances to calcine, in nitrogen
Under gas atmosphere protection, it is warming up to the rate of 3 DEG C/min and keeps the temperature 1 hour at 1150 DEG C and obtain pre-composite porous current collector；Finally
It puts it into pre-configured dilute hydrochloric acid solution and impregnates 10 hours, then is remaining to remove with the flushing of a large amount of deionized waters
Hydrochloric acid.Finally drying obtains compound porous collector in 80 DEG C of convection oven.It is direct with prepared compound porous collector
The assembling of button cell is carried out as electrode slice.Relative to plane copper collector, using compound porous afflux prepared by the present invention
Body more efficiently the growth of dendrite inhibition and can prevent the short circuit of battery in charge and discharge process.
Embodiment 3
It takes 7g copper powders to be placed in mortar, 2g calcium oxide is added, then adds 1g metal magnesium powder, is sufficiently mixed, when grinding
Between about 1.5 hours.It weighs 0.25g mixed-powder again later, is added in the mold that diameter is 12mm, pressure is 25Mpa progress
Compacting, retention time are 3 minutes；Then the disk pressed high temperature process furnances are put into calcine, under argon atmosphere protection,
It is warming up to the rate of 10 DEG C/min and keeps the temperature 1.5 hours at 1300 DEG C and obtain pre-composite porous current collector；It finally puts it into pre-
It first impregnates 15 hours in configured dilute hydrochloric acid solution, then is rinsed with a large amount of deionized waters to remove remaining hydrochloric acid.Finally
It is dried in 60 DEG C of convection oven, compound porous collector can be obtained.With prepared compound porous collector directly as
The assembling of electrode slice progress button cell.It, can using compound porous collector prepared by the present invention relative to plane copper collector
To realize be more good chemical property.
Embodiment 4
It takes 4g copper powders to be placed in mortar, 1.5g calcium carbonate is added, then add 1g magnesium oxide powder, is sufficiently mixed, grind
Time about 2 hours.It weighs 0.16g mixed-powder again later, is added in the mold that diameter is 12mm, pressure is 35Mpa progress
Compacting, retention time are 2 minutes；Then the disk pressed high temperature process furnances are put into calcine, under argon atmosphere protection,
It is warming up to the rate of 5 DEG C/min and keeps the temperature 2 hours at 1250 DEG C and obtain pre-composite porous current collector；It finally puts it into and matches in advance
It impregnates 12 hours in the dilute hydrochloric acid solution set, then is rinsed with a large amount of deionized waters to remove remaining hydrochloric acid.Finally 50
DEG C convection oven in drying obtain compound porous collector.It is detained with compound porous collector is prepared directly as electrode slice
The assembling of formula battery.Relative to plane copper collector, can more effectively be pressed down using compound porous collector prepared by the present invention
The growth of Li dendrite processed.
Claims (7)
1. a kind of preparation method of the compound porous collector for lithium an- ode protection, the compound porous collector include
Three-dimensional porous copper skeleton as main body and the close lithium active material that is supported on copper skeleton；Preparation method includes following step
It is rapid:
(1) a certain proportion of copper powder, pore creating material, close lithium active material powder are weighed uniformly to mix, obtains mixed-powder；It is described mixed
It closes in powder, the mass content of pore creating material is 10-30wt%, and the mass content of close lithium active material is 10-20wt%, and surplus is
Copper powder；
(2) mixed-powder that appropriate step (1) obtains is weighed, tabletting is carried out with mold, obtains thin layer disk, then in protection gas
It is warming up to 1100-1500 DEG C with the rate of 3-10 DEG C/min under atmosphere, calcination processing 1-4h is kept the temperature, obtains pre-composite porous afflux
Body；
(3) obtained pre-composite porous current collector is soaked in the dilute hydrochloric acid of 5-15% to remove pore creating material, is then spent again
Ionized water removes remaining hydrochloric acid, is placed in 50-80 DEG C of baking oven and is dried, compound porous collector can be obtained.
2. preparation method as described in claim 1, it is characterised in that: the close lithium active material be Zn, Mg, Al, Si,
ZnO、MgO、Al2O3Or SiO2One of or any several combination.
3. preparation method as claimed in claim 1 or 2, it is characterised in that: the pore creating material is calcium oxide, calcium carbonate or carbon
Sour sodium.
4. preparation method as claimed in claim 3, it is characterised in that: the content of pore creating material is 10- in the mixed-powder
20wt%.
5. preparation method as claimed in claim 3, it is characterised in that: in step (2), calcination temperature is forged at 1100-1400 DEG C
The burning time is 2-4h.
6. preparation method as claimed in claim 1 or 5, it is characterised in that: in step (2), when calcining protective atmosphere be argon gas,
The combination of one or both of nitrogen arbitrary proportion.
7. the preparation method according to claim 1 compound porous collector obtained for lithium an- ode protection.
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| CN201810701013.XA CN109103456B (en) | 2018-06-29 | 2018-06-29 | Preparation method of composite porous current collector for lithium metal negative electrode protection |
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| CN201810701013.XA CN109103456B (en) | 2018-06-29 | 2018-06-29 | Preparation method of composite porous current collector for lithium metal negative electrode protection |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109807350A (en) * | 2019-03-06 | 2019-05-28 | 浙江工业大学 | A kind of preparation method of 3-D ordered multiporous copper current collector |
| CN111180671A (en) * | 2019-10-08 | 2020-05-19 | 南京宁智高新材料研究院有限公司 | Preparation process of framework-supported metal lithium electrode with double coatings and high specific surface area |
| CN112103472A (en) * | 2019-06-17 | 2020-12-18 | 上海汽车集团股份有限公司 | Metal lithium composite material and preparation method thereof |
| CN113130881A (en) * | 2021-04-12 | 2021-07-16 | 肇庆市华师大光电产业研究院 | Preparation method of lithium-sulfur battery cathode material |
| CN113540409A (en) * | 2021-07-15 | 2021-10-22 | 四川启睿克科技有限公司 | Adjustable lithium-free negative electrode and preparation method thereof |
| CN115275212A (en) * | 2022-08-10 | 2022-11-01 | 哈尔滨工业大学 | Preparation method of copper-based current collector of anode-free lithium ion battery |
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| CN111180671A (en) * | 2019-10-08 | 2020-05-19 | 南京宁智高新材料研究院有限公司 | Preparation process of framework-supported metal lithium electrode with double coatings and high specific surface area |
| CN113130881A (en) * | 2021-04-12 | 2021-07-16 | 肇庆市华师大光电产业研究院 | Preparation method of lithium-sulfur battery cathode material |
| CN113540409A (en) * | 2021-07-15 | 2021-10-22 | 四川启睿克科技有限公司 | Adjustable lithium-free negative electrode and preparation method thereof |
| CN115275212A (en) * | 2022-08-10 | 2022-11-01 | 哈尔滨工业大学 | Preparation method of copper-based current collector of anode-free lithium ion battery |
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