CN110350200A - A kind of lithium ion battery three-dimensional Arrays of Copper Nanowires collector and preparation method thereof - Google Patents
A kind of lithium ion battery three-dimensional Arrays of Copper Nanowires collector and preparation method thereof Download PDFInfo
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- CN110350200A CN110350200A CN201810287352.8A CN201810287352A CN110350200A CN 110350200 A CN110350200 A CN 110350200A CN 201810287352 A CN201810287352 A CN 201810287352A CN 110350200 A CN110350200 A CN 110350200A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/34—Anodisation of metals or alloys not provided for in groups C25D11/04 - C25D11/32
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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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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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- 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
- H01M4/70—Carriers or collectors characterised by shape or form
- H01M4/75—Wires, rods or strips
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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
This application discloses a kind of lithium ion battery three-dimensional Arrays of Copper Nanowires collectors and preparation method thereof, belong to battery material field.The three-dimensional Arrays of Copper Nanowires collector of the lithium ion battery, the nano wire are distributed in copper foil surface, and the diameter of the nano wire is 1-5nm, and the length of nano wire is 5-15nm.The three-dimensional Arrays of Copper Nanowires collector of lithium ion battery provided herein, lithium ion battery is big with the surface area of three-dimensional Arrays of Copper Nanowires collector, and the lithium ion battery of preparation is light-weight, and functional, cycle-index is more, long service life.The preparation method is simple, the specific surface area of superelevation, and the structural homogeneity of copper nano-wire is good, reproducible.
Description
Technical field
This application involves a kind of lithium ion battery three-dimensional Arrays of Copper Nanowires collectors and preparation method thereof, belong to battery
Material Field.
Background technique
Copper aluminium foil good conductivity, quality is soft, cheap.It is known that lithium battery working principle is to turn chemical energy
A kind of a kind of electrochemical appliance for turning to electric energy, then in this process, it would be desirable to electric energy that medium converts chemical energy
It passes out, just needs conductive material here.And in common material, metal material is the best material of electric conductivity and in gold
Belonging in material that cheap electric conductivity is again good is exactly copper foil and aluminium foil.Meanwhile in lithium battery, we mainly have winding and fold
Two kinds of processing methods of piece.For winding, the pole piece for needing to be used to prepare battery has certain flexibility, just can guarantee
Pole piece winding when brittle failure does not occur the problems such as, and metal material in, copper aluminium foil is also the softer metal of quality.Finally it is exactly
Consider battery preparation cost, comparatively, copper aluminium foil price is relatively cheap, and copper and aluminium element are resourceful in the world.
For lithium ion battery, usually used plus plate current-collecting body is aluminium foil, and negative current collector is copper foil, in order to protect
Collector is demonstrate,proved in inside battery stability, the two purity is required 98% or more.With the continuous development of lithium power technology, no matter
It is the battery of the lithium battery or electric car for digital product, the energy density that we are intended to battery is high as far as possible, battery
Weight it is more and more lighter, and main in collector this block is exactly the thickness and weight for reducing collector, is intuitively reduced
The volume and weight of battery.
Summary of the invention
According to the one aspect of the application, a kind of three-dimensional Arrays of Copper Nanowires collector of lithium ion battery, lithium are provided
Ion battery is big with the surface area of three-dimensional Arrays of Copper Nanowires collector, light-weight, the property of the battery of the lithium ion battery of preparation
Can be good, cycle-index is more, long service life.
The three-dimensional Arrays of Copper Nanowires collector of the lithium ion battery, which is characterized in that the nano wire is distributed in copper foil
Surface, the diameter of the nano wire are 1-5nm, and the length of nano wire is 5-15nm.
Preferably, the nano wire is evenly distributed on copper foil surface, and the diameter of the nano wire is 2-54nm, nano wire
Length is 7-12nm.
According to the one aspect of the application, a kind of method of above-mentioned three-dimensional Arrays of Copper Nanowires collector, the party are provided
Method preparation is simple, environmental protection and energy saving.
This prepares the method for three-dimensional Arrays of Copper Nanowires collector described in claim 1, which is characterized in that including following
Step:
1) electrolyte is the lye of deoxygenation, and the temperature for controlling electrolyte is 15-55 DEG C, using copper as anode；
2) control first stage current density is 1.0~2.0mA/cm2, the time is 2~10min；
3) control second stage current density is 2.0~4.5mA/cm2, the time is 5~25min；
4) it in the film of copper Surface Creation blue, wash with distilled water and dries, after thermal reduction, obtains three-dimensional copper nano-wire
Array collector.
Preferably, the temperature of the electrolyte is 20-50 DEG C.
Preferably, the first stage current density is 1.2~1.8mA/cm2。
Preferably, the first stage current time is 4~8min.
Preferably, the second stage current density is 2.2~4.3mA/cm2。
Preferably, the second stage current time is 7~23min.
Preferably, it is described thermal reduction step be 170~195 DEG C at a temperature of heat-treat 12~18h.
Preferably, the pre-treatment step of the anode copper is that 3~5min is impregnated in the hydrochloric acid for be put into 0.5~1.8mol/L,
Cleaning, it is spare after dry.
Preferably, the method for above-mentioned three-dimensional Arrays of Copper Nanowires collector includes the following steps:
1) using red copper as anode, sodium hydroxide solution or potassium hydroxide solution are electrolyte, and stainless steel is cathode, are saturated chlorine
Change mercurous electrode is reference electrode, is first passed through inert gas removal oxygen in electrolytic cell within the scope of 5~60 DEG C, then controls
Current density is 0.5~5mA/cm2, 4~30min of anodic oxidation, in the Cu (OH) of red copper surface generation blue2Film, with steaming
Distilled water is cleaned and is dried, and Cu (OH) is obtained2Nano-wire array；
2) by Cu (OH)2Nano-wire array is placed in nitrogen atmosphere, in 160~200 DEG C of reactor, thermal reduction 10~
20h, then room temperature is naturally cooled to, three-dimensional copper nano-wire battle array collector can be obtained.
Preferably, the method for above-mentioned three-dimensional Arrays of Copper Nanowires collector further include: red copper is first put into 0.1~2mol/L
Hydrochloric acid in impregnate 3~5min, then wash with distilled water, then cleaned with ethyl alcohol, it is spare after dry；
The concentration of the sodium hydroxide solution or potassium hydroxide solution is 0.1~4mol/L.
The beneficial effect that the application can generate includes:
1) the three-dimensional Arrays of Copper Nanowires collector of lithium ion battery provided herein, the three-dimensional copper of lithium ion battery
The surface area of nano-wire array collector is big, the lithium ion battery of preparation it is light-weight, functional, cycle-index is more, use
Service life is long.
2) the lithium ion battery provided herein preparation method of three-dimensional Arrays of Copper Nanowires collector, has letter
Single, the structural homogeneity of the specific surface area of superelevation, copper nano-wire is good, reproducible.
Specific embodiment
The application is described in detail below with reference to embodiment, but the application is not limited to these embodiments.
Unless otherwise instructed, the raw material in embodiments herein and catalyst are bought by commercial sources.
1 bronze medal of embodiment receives the preparation of line collector
1) copper sheet of 2.0 × 2.0cm is impregnated into the oxide that 5min goes to copper removal surface with the hydrochloric acid solution of 1.2M, then divided
It is not cleaned with distilled water and ethyl alcohol, it is spare after dry；
2) anode is copper sheet, and cathode is stainless steel substrates, and reference electrode is saturation calomel electrode, reference electrode electrolyte
The NaOH solution for being 2M for concentration；
3) at 25 DEG C, then electrolyte controls first stage constant current density 1.5mA/cm after deoxygenation2,
Time is 6min；Control second stage current density is 3.5mA/cm2, time 15min；
4) in the Cu (OH) of copper sheet Surface Creation blue2Film is dried for standby wash with distilled water；
5) by Surface Creation blue Cu (OH)2The copper sheet of film is put into tubular sealed furnace, is passed through H2, heating rate 2.5
DEG C/min, in 178 DEG C of thermal reduction 15h, then room temperature is naturally cooled to get three-dimensional Arrays of Copper Nanowires collector is arrived.
Gained sample carries out surface sweeping Electronic Speculum characterization, shows in electron microscope, uniform nanowire growth obtains in copper sheet substrate
Line collector is received with copper to lithium ion battery.
The three-dimensional copper of embodiment 2 receives the Electrochemical Characterization test of linear array collector
Lithium ion battery prepared by embodiment 1 is received into line collector with copper and is used to load lithium ion battery anode material, i.e.,
In one layer of metallic tin (Sn) film of collection liquid surface electro-deposition.Electrodeposition condition: plating solution is 0.05M SnSO4With 1.5M H2SO4
Mixed solution, constant potential -1.0V (saturation calomel electrode be reference electrode), sedimentation time 30S.
In contrast, in bright one layer of Sn film of the direct electro-deposition in copper sheet surface.Electrodeposition condition: plating solution 0.05M
SnSO4With 1.5M H2SO4Mixed solution, constant potential -1.0V (saturation calomel electrode be reference electrode), sedimentation time
120S。
The copper sheet that electro-deposition has Sn film is cut into the sequin that diameter is about 14mm, is being directly used as lithium ion battery just
Pole, metal lithium sheet are used as cathode, and electrolyte is by LiPF6, ethylene carbonate and diethyl carbonate composition (LiPF in electrolyte6Concentration
For 1M, the volume ratio of ethylene carbonate and diethyl carbonate is 1: 1), diaphragm is Celgard2400 microporous polypropylene membrane, is being filled
2025 type button cells are assembled into the glove box of full argon gas.
Charge-discharge test, the three-dimensional Arrays of Copper Nanowires collector base Sn of lithium ion battery are carried out to 2025 type button cells
The discharge cycles curve graph of film, 1C=994mA/g, voltage window 2.0-0.02V, discharge capacity is 1558.4mAh/ for the first time
G, capacity is 882.4mAh/g, capacity retention ratio 56.6% after recycling 50 times；
The discharge cycles of bright copper sheet base Sn film are bent, and discharge capacity is 1290.7mAh/g for the first time, hold after circulation 30 times
Amount is 211.9mAh/g, capacity retention ratio 21.3%.Obviously, lithium ion battery Arrays of Copper Nanowires collector is for loading
Lithium ion battery negative material Sn film has better charge-discharge performance.
The preparation of the three-dimensional Arrays of Copper Nanowires collector of embodiment 3
1) copper belt of 1.5 × 1.5cm is first impregnated with the hydrochloric acid solution of 0.1M to the oxide for going to copper removal surface for 3 minutes,
Then wash with distilled water 5 times, then cleaned 3 times with ethyl alcohol, it is spare after dry；The KOH solution or NaOH that configuration concentration is 2M are molten
Liquid is spare.
2) using copper belt as anode, 304 stainless steel substrates be cathode, saturation calomel electrode be reference electrode, anode and
The KOH solution or NaOH solution of cathode spacing about 3cm, 2M are electrolyte, and at 25 DEG C, inert gas is first passed through in electrolytic cell
(high-purity N2Or Ar2Deng) about 30min remove O2, then control constant current density 2.5mA/cm2, the anodic oxidation time
12min, in the Cu (OH) of copper belt Surface Creation blue2Film 3 times wash with distilled water, is dried for standby.
3, by Surface Creation blue Cu (OH)2The copper belt of film is put into reactor --- in tubular sealed furnace, be passed through by
The H that hydrogen generator generates2, 3 DEG C/min of heating rate in 180 DEG C of thermal reduction 20h, then naturally cools to room temperature, copper belt table
The film of face blue is transformed into wine-colored Cu nano-wire array.Gained sample carries out surface sweeping Electronic Speculum (SEM) characterization, and uniform receives
Nanowire arrays are grown on the copper-based bottom of copper belt, obtain the three-dimensional Arrays of Copper Nanowires collector of lithium ion battery.
The Electrochemical Characterization test of the three-dimensional Arrays of Copper Nanowires collector of embodiment 4
2 lithium ion battery of embodiment is used to load anode of lithium ion battery material with three-dimensional Arrays of Copper Nanowires collector
Material, i.e., in one layer of metallic tin (Sn) film of collection liquid surface electro-deposition.Electrodeposition condition: plating solution is 0.05M SnSO4And 1.5M
H2SO4Mixed solution, constant potential -1.0V (saturation calomel electrode be reference electrode), sedimentation time 30S.
In contrast, bright one layer of Sn film of the direct electro-deposition of red copper belt surface (.Electrodeposition condition: plating solution is
0.05M SnSO4With 1.5M H2SO4Mixed solution, constant potential -1.0V (saturation calomel electrode be reference electrode) sinks
Product time 120S.
The copper belt that electro-deposition has Sn film is cut into the sequin that diameter is about 14mm, is directly used as lithium ion battery
Anode, metal lithium sheet are used as cathode, and electrolyte is by LiPF6, ethylene carbonate and diethyl carbonate composition (LiPF in electrolyte6It is dense
Spending is 1M, and the volume ratio of ethylene carbonate and diethyl carbonate is 1: 1), diaphragm is Celgard2400 microporous polypropylene membrane,
2025 type button cells are assembled into glove box full of argon gas.
Charge-discharge test, the three-dimensional Arrays of Copper Nanowires collector base Sn of lithium ion battery are carried out to 2025 type button cells
The discharge cycles curve graph (1C=994mA/g, voltage window 2.0-0.02V) of film, discharge capacity is for the first time
1337.2mAh/g, capacity is 441.2mAh/g, capacity retention ratio 40.4% after recycling 30 times；Bright red copper tape base Sn is thin
The discharge cycles curve of film, discharge capacity is 1290.7mAh/g for the first time, and capacity is 211.9mAh/g after circulation 30 times, and capacity is protected
Holdup is 21.3%.Obviously, the three-dimensional Arrays of Copper Nanowires collector of lithium ion battery is for loading negative electrode of lithium ion battery material
Expect that Sn film has better charge-discharge performance.
The above is only several embodiments of the application, not does any type of limitation to the application, although this Shen
Please disclosed as above with preferred embodiment, however not to limit the application, any person skilled in the art is not taking off
In the range of technical scheme, a little variation or modification are made using the technology contents of the disclosure above and is equal to
Case study on implementation is imitated, is belonged in technical proposal scope.
Claims (10)
1. a kind of three-dimensional Arrays of Copper Nanowires collector of lithium ion battery, which is characterized in that nano wire is distributed in copper foil surface,
The diameter of the nano wire is 1-5nm, and the length of nano wire is 5-15nm.
2. three-dimensional Arrays of Copper Nanowires collector according to claim 1, which is characterized in that the nano wire is uniformly distributed
In copper foil surface, the diameter of the nano wire is 2-54nm, and the length of nano wire is 7-12nm.
3. a kind of method for preparing three-dimensional Arrays of Copper Nanowires collector described in claim 1, which is characterized in that including following
Step:
1) electrolyte is the lye of deoxygenation, and the temperature for controlling electrolyte is 15-55 DEG C, using copper as anode；
2) control first stage current density is 1.0~2.0mA/cm2, the time is 2~10min；
3) control second stage current density is 2.0~4.5mA/cm2, the time is 5~25min；
4) it in the film of copper Surface Creation blue, wash with distilled water and dries, after thermal reduction, obtains three-dimensional Arrays of Copper Nanowires
Collector.
4. according to the method described in claim 3, it is characterized in that, the temperature of the electrolyte is 20-50 DEG C.
5. according to the method described in claim 3, it is characterized in that, the first stage current density is 1.2~1.8mA/cm2,
First stage current time is 4~8min.
6. according to the method described in claim 3, it is characterized in that, the second stage current density is 2.2~4.3mA/cm2,
The second stage current time is 7~23min.
7. according to the method described in claim 3, it is characterized in that, it is described thermal reduction step be 170~195 DEG C at a temperature of
Heat-treat 12~18h.
8. according to the method described in claim 3, it is characterized in that, the pre-treatment step of the anode copper be put into 0.5~
3~5min is impregnated in the hydrochloric acid acid of 1.8mol/L, cleaning is spare after dry.
9. according to the method described in claim 3, it is characterised in that it includes following step:
1) using red copper as anode, sodium hydroxide solution or potassium hydroxide solution are electrolyte, and stainless steel is cathode, are saturated protochloride
Mercury electrode is reference electrode, is first passed through inert gas removal oxygen in electrolytic cell within the scope of 5~60 DEG C, then controls electric current
Density is 0.5~5mA/cm2, 4~30min of anodic oxidation, in the Cu (OH) of red copper surface generation blue2Film uses distilled water
It cleans and dries, obtain Cu (OH)2Nano-wire array；
2) by Cu (OH)2Nano-wire array is placed in nitrogen atmosphere, in 160~200 DEG C of reactor, heat-treats 10~20h, then
Room temperature is naturally cooled to, three-dimensional copper nano-wire battle array collector can be obtained.
10. according to the method described in claim 3, it is characterized by further comprising: red copper to be first put into the salt of 0.1~2mol/L
3~5min is impregnated in acid, then wash with distilled water, then is cleaned with ethyl alcohol, it is spare after dry；
The concentration of the sodium hydroxide solution or potassium hydroxide solution is 0.1~4mol/L.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111668493A (en) * | 2020-06-16 | 2020-09-15 | 南开大学 | Three-dimensional current collector for inhibiting dendritic crystal of lithium metal negative electrode and application of three-dimensional current collector in metal lithium battery |
| CN112054176A (en) * | 2020-09-10 | 2020-12-08 | 北京航空航天大学 | Self-repairing lithium ion battery anode material and preparation method thereof |
| CN112838216A (en) * | 2020-11-16 | 2021-05-25 | 河北零点新能源科技有限公司 | Method for changing color of copper foil of current collector of lithium ion battery |
| CN113488607A (en) * | 2021-06-07 | 2021-10-08 | 暨南大学 | Preparation and application of metal zinc cathode with functional nano material modification layer |
| CN114243027A (en) * | 2021-12-17 | 2022-03-25 | 广东工业大学 | Sodium ion battery negative current collector, preparation method thereof and sodium ion battery |
| CN114850488A (en) * | 2022-05-06 | 2022-08-05 | 中国科学技术大学 | Preparation method of biomass-derived copper nanowire and preparation method of copper current collector |
| CN115172761A (en) * | 2022-09-08 | 2022-10-11 | 深圳市汉嵙新材料技术有限公司 | Composite copper-based current collector and preparation method thereof, battery electrode and lithium ion battery |
| CN115566203A (en) * | 2022-10-24 | 2023-01-03 | 哈尔滨师范大学 | Copper nanowire array electrode connected in series with cobalt nitrogen carbon hollow structure and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111668493A (en) * | 2020-06-16 | 2020-09-15 | 南开大学 | Three-dimensional current collector for inhibiting dendritic crystal of lithium metal negative electrode and application of three-dimensional current collector in metal lithium battery |
| CN112054176A (en) * | 2020-09-10 | 2020-12-08 | 北京航空航天大学 | Self-repairing lithium ion battery anode material and preparation method thereof |
| CN112838216A (en) * | 2020-11-16 | 2021-05-25 | 河北零点新能源科技有限公司 | Method for changing color of copper foil of current collector of lithium ion battery |
| CN113488607A (en) * | 2021-06-07 | 2021-10-08 | 暨南大学 | Preparation and application of metal zinc cathode with functional nano material modification layer |
| CN113488607B (en) * | 2021-06-07 | 2022-05-06 | 暨南大学 | Preparation and application of metal zinc cathode with functional nano material modification layer |
| CN114243027A (en) * | 2021-12-17 | 2022-03-25 | 广东工业大学 | Sodium ion battery negative current collector, preparation method thereof and sodium ion battery |
| CN114243027B (en) * | 2021-12-17 | 2024-02-13 | 广东工业大学 | Negative current collector of sodium ion battery, preparation method of negative current collector and sodium ion battery |
| CN114850488A (en) * | 2022-05-06 | 2022-08-05 | 中国科学技术大学 | Preparation method of biomass-derived copper nanowire and preparation method of copper current collector |
| CN115172761A (en) * | 2022-09-08 | 2022-10-11 | 深圳市汉嵙新材料技术有限公司 | Composite copper-based current collector and preparation method thereof, battery electrode and lithium ion battery |
| CN115172761B (en) * | 2022-09-08 | 2022-11-22 | 深圳市汉嵙新材料技术有限公司 | Composite copper-based current collector, preparation method thereof, battery electrode and lithium ion battery |
| CN115566203A (en) * | 2022-10-24 | 2023-01-03 | 哈尔滨师范大学 | Copper nanowire array electrode connected in series with cobalt nitrogen carbon hollow structure and preparation method and application thereof |
| CN115566203B (en) * | 2022-10-24 | 2024-01-26 | 哈尔滨师范大学 | Copper nanowire array electrode with cobalt-nitrogen-carbon hollow structure in series connection and preparation method and application thereof |
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