CN105449271B - A kind of CuS is the aluminium ion secondary cell and its preparation process of anode - Google Patents
A kind of CuS is the aluminium ion secondary cell and its preparation process of anode Download PDFInfo
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- CN105449271B CN105449271B CN201610005992.6A CN201610005992A CN105449271B CN 105449271 B CN105449271 B CN 105449271B CN 201610005992 A CN201610005992 A CN 201610005992A CN 105449271 B CN105449271 B CN 105449271B
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M10/058—Construction or manufacture
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
-
- 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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention belongs to aluminium ion secondary cells and its preparation process that new green energy battery technology field more particularly to a kind of CuS material are anode.Wherein cathode active material is CuS, and anode is metallic aluminium or aluminium-containing alloy, and liquid ion electrolyte is to contain Al3+The nonaqueous solution electrolysis liquid of ion assembles battery plus-negative plate and its electrolyte etc. using the Soft Roll package or cylindrical container of insulation.Aluminium ion secondary cell provided by the present invention can be repeatedly charged and discharged, have high capacity, good cycling stability, and raw material are cheap and environmental-friendly, and first circle charging and discharging capacity is respectively 270mAhg‑1With 275mAh g‑1, discharge platform is up to 1.15Vvs.Al3+/Al.The aluminium ion secondary cell can be widely applied to the various fields such as electronic industry, communication industry.
Description
Technical field
The invention belongs to the aluminium ions that new green energy battery technology field more particularly to a kind of CuS material are anode
Secondary cell and its preparation process.
Background technique
As economy is advanced by leaps and bounds, energy crisis and environmental pollution increasingly sharpen.Therefore, a kind of renewable energy is developed
Source, as energy-storage battery becomes the hot spot of current research.Lithium ion battery based on carbonaceous material, such as using graphite as anode,
With lithium metal oxide material (LiCoO2Deng) it is used as cathode, it is always portable using aprotic liquids as the battery of electrolyte
Hot spot in the scientific research of formula electronic application field.But since the limitation of lithium resource leads to expensive and biggish peace
Full hidden danger limits the further development of lithium ion battery.In order to meet smaller, lighter, safer electronic application new demand,
Increase in demand to the lower secondary cell such as its operating voltage, cyclical stability, energy density, security performance and cost.With
Lithium is compared, and aluminium is the most abundant metal of present on earth amount, and crustal abundance occupies third.Aluminium ion rechargeable battery exchanges trivalent
Al3+, therefore its specific capacity has very big potentiality to be exploited.Further, since it is with lower reactivity, so aluminium ion battery
Great amount of cost can be saved and greatly improve battery safety.To which the multivalent ion battery based on aluminium ion deintercalation is expected to use
In extensive energy storage device.
Jayaprakash, which is equal to 2011, uses transition metal oxide V2O5As the positive electrode of aluminium ion battery,
(document: Jayaprakash N, Das S K, Archer L A. The rechargeable aluminum-ion
Battery [J] Chem. Commun., 2011,47 (47): 12610-12612).The specific volume the study found that its first circle discharges
Amount is about 300 mAh g-1, 20 circle after 270 mAh g of residue-1, but its discharge potential is only 0.55 Vvs. Al3+/Al。
Liu et al. equally used TiO in 20122Positive electrode of the metal oxide as aluminium ion battery, (document: Liu S, Hu J
J, Yan N F, et al. Aluminum storage behavior of anatase TiO2 nanotube arrays
in aqueous solution for aluminum ion batteries[J]. Energy Environ. Sci.,
2012,5 (12): 9743-9746), research finds that its discharge potential is relatively low, only 0.67 Vvs. Al3+/Al, and recycle
After 15 circles, specific capacity is only 70 mAh g-1.Jiao Shu is equal by force to apply for Chinese invention patent No. in 2014
CN201410419495.1 reports the positive electrode using graphite-like carbonaceous material as aluminium ion battery, and rafifinal is cathode
A kind of rechargeable aluminium ion secondary battery of material.And Chinese invention patent No. is applied in 2015
CN201510188866.4 reports soft as the aluminium ion of aluminium ion secondary battery positive electrode material using graphite-structure carbon material
The preparation process of packet battery.The seminar has carried out a large amount of correlative study to this series material and technique and has worked, using carbon
Paper is as aluminium ion cell positive material, and after circulation 100 is enclosed, remaining specific capacity is up to 67 mAh g-1, and have higher follow
Ring stability (document: Sun H, Wang W, Yu Z, et al. A new aluminium-ion battery with
high voltage, high safety and low cost[J]. Chem. Commun., 2015, 51(59):
11892-11895).Recently, be published on " Nature " magazine one of the Dai et al. of Stanford University is entitled " a kind of ultrafast
The article of rechargeable aluminium ion battery " causes extensive concern (document: Lin M C, Gong M, Lu B, et again
Al. An ultrafast rechargeable aluminium-ion battery [J] Nature, 2015), research is adopted
Pyrolytic graphite and 3 is used to tie up graphite foam as aluminium ion cell positive material, specific capacity is stablized in 60 mAh g-1More than.But
It is that patent and document so far has not been reported about CuS and its composite material as anode and with the aluminium ion of this anode
Secondary cell.
Summary of the invention
The purpose of the present invention is to provide a kind of novel aluminum ion secondary batteries that may replace lithium ion battery, i.e. stability
Good, first circle specific discharge capacity is high, and discharge platform is high, and the CuS for having higher cyclic reversibility is the secondary electricity of aluminium ion of anode
Pond and its preparation process.
To achieve the above object, the present invention is the following technical schemes are provided: a kind of CuS is the aluminium ion secondary cell of anode,
The aluminium ion secondary cell includes anode, battery cathode, the liquid of nonaqueous solution electrolysis containing aluminium ion, inert metal paillon afflux
Body, diaphragm, lead and battery case, which is characterized in that the material of the anode includes micron order or nanoscale CuS, conductive material
And binder.
Further, the mass percent of the CuS is 60-90%, the mass percent of conductive material is 10-40% and bonding
Agent mass percent is 0-10%.
Further, the conductive material is carbonaceous material or metal paste, and the carbonaceous material includes acetylene black, graphite
Alkene, amorphous carbon, conductive carbon black or super carbon；The metal paste includes platinum slurry or silver paste.
Further, when the conductive material is graphene, the mass fraction of conductive material is 10-20%, the quality point of CuS
Number is 70-85%, and the mass fraction of binder is 5-10%；The conductive material is acetylene black, agraphitic carbon, conductive carbon black or super
When grade carbon, the mass fraction of conductive material is 20-50%, and the mass fraction of CuS is 40-75%, and the mass fraction of binder is 5-
10%；When the conductive material is metal paste, the mass fraction of conductive material is 10-40%, and the mass fraction of CuS is 60-
90%。
Further, the binder is the mixture of one or both of Kynoar or polytetrafluoroethylene (PTFE).
Further, the negative electrode material be metallic aluminium of the purity greater than 90% or metallic aluminium and copper, iron, nickel, lead, bismuth, tin,
The alloy that silver is formed.
It further, include aluminum halide and ionic liquid, the aluminum halide and ion in the non-aqueous electrolyte containing aluminium
The molar ratio of liquid is 0.4:1-2.4:1.
Further, the anion of the ionic liquid includes F-, Cl-, Br-, I-, PF6-, CN-, SCN-, [N (CF3SO2)]-Or
[N(CN)2]-Ion；Cation include imidazoles drone ion, pyridinium ion, pyrroles's drone ion, piperidines drone ion, morpholine drone from
Son, quaternary ammonium salt ion, quaternary phosphonium salt ion or tertiary sulfosalt ion.
It is a further object of the present invention to provide the preparation steps for the aluminium ion secondary cell that above-mentioned CuS is anode, including with
Under preparation step:
Step 1: including that micron order or nanoscale CuS, conductive material, binder proportionally weigh uniformly respectively by raw material
Mixing, is dried to gelling material, the inert metal for being then uniformly applied to gelling material in 60-100 degrees Celsius of baking oven
On collector, it is made with a thickness of 0.1-1mm sheet composite positive pole, composite positive pole diaphragm is wrapped up to get to just
Pole material；
Step 2: by with a thickness of the metal aluminum or aluminum alloy of 0.1-1mm, after fine sandpaper polishing cleaning, drying is to get arriving
Negative electrode material；
Step 3: aluminum halide and ionic liquid are mixed in the glove box of ar gas environment with molar ratio for 0.4:1-2.4:1
It closes, stand 24 hours or more, that is, it is configured to containing the liquid of nonaqueous solution electrolysis containing aluminium ion that can move freely；
Step 4: positive electrode and step 2 that step 1 obtains finally are obtained into negative electrode material and step 3 obtains containing aluminium from
Sub- nonaqueous solution electrolysis liquid is assembled into glove box, obtains Soft Roll aluminium ion battery Soft Roll or tubular battery, i.e. CuS is positive
The aluminium ion secondary cell of pole；
Step 5: after battery pack installs, carrying out charge-discharge test again after liquid whole wetting electrode piece to be electrolysed.
Further, in step 1, the diaphragm be MIcroporous polyolefin film diaphragm material, polyethylene micropore diaphragm material and
One of glass fiber material；The inert metal collector includes tantalum piece, niobium sheet, molybdenum sheet, titanium sheet, nickel foam or gold and platinum
Race's metal.
The beneficial effects of the present invention are: due to the adoption of the above technical scheme, the present invention uses CuS material as positive material
Material, metallic aluminium or aluminium-containing alloy constitute a kind of chargeable aluminium ion battery as negative electrode material.Since the present invention is to positive and negative
Pole material, diaphragm, collector and its electrolyte etc. have carried out fine selection by experimental study, and combine strict preparation side
Method, so the invention has the characteristics that: propose a kind of novel multivalent ion battery, i.e. aluminium ion battery system；Due to aluminium
Element the earth's crust rich reserves, it is cheap, greatly reduce the preparation cost of battery, while also improving ion battery
Security performance；CuS is readily synthesized, at low cost, nontoxic, so having a wide range of applications in terms of electrochemical energy storage；
Diaphragm have good insulation performance, to electrolyte ion have good transparent performance, have preferable chemical stability and
Electrochemical stability；Aluminium ion electrolyte, conductivity is high, and thermal stability is good, with positive and negative pole material, diaphragm and binder in battery
Deng not chemically reacting；Using CuS material, its first circle specific discharge capacity is up to 275 mAh g-1, discharge platform is up to 1.15 Vvs. Al3+/Al, and have higher cyclic reversibility, aluminium ion battery of the invention can be applied to various fields, such as electronics work
Industry, communication industry, electric car etc..
Detailed description of the invention
Fig. 1 is aluminium ion secondary cell first lap charge-discharge test curve prepared by embodiment 1；
Fig. 2 is 15 circle cycle performance curves before aluminium ion secondary cell prepared by embodiment 1.
Specific embodiment
The present invention will be described in more detail below by specific embodiment, but protection scope of the present invention is not limited
In these embodiments.
[embodiment 1]
Positive active material is CuS, and conductive material is acetylene black, and binder is polytetrafluoroethylene (PTFE).Three according to
Mass ratio is that the ratio of 50:40:10 is dried to gelling material in 80 degrees Celsius of baking oven after mixing in dehydrated alcohol, so
Gelling material is uniformly applied to afterwards on sizeable collector tantalum piece (thickness 0.01mm), is finally dried at 100 degrees Celsius
Use GF/D diaphragm material package as anode after drying in case standing 12 hours or more.Cathode uses thick with a thickness of 0.2mm
High-purity aluminium flake is cut into sizeable, is then polished with fine sandpaper and is cleaned in dehydrated alcohol, and ultrasonic vibration
Negative electrode material is used as after drying.It is in molar ratio 1.3:1 in argon gas by anhydrous aluminum chloride and 1- ethyl-3-methylimidazole chloride
It is configured to ionic liquid in the glove box of environment, as aluminium ion secondary cell electrolyte of the invention.It finally will be ready
Positive plate, negative electrode tab and electrolyte are assembled into Soft Roll aluminium ion battery in glove box.After battery installs 24 hours, in 0.1-
Charge-discharge test is carried out between 2.0V.When using CuS material as aluminium ion secondary battery anode active compound material, first circle
Specific discharge capacity is up to 275 mAh g-1, discharge platform is up to 1.15 Vvs. Al3+/Al, and have preferable cycle performance,
See attached drawing 1.Its specific capacity there remains 160 mAh g after 15 circle of circulation-1, and stability is continuously improved, and sees attached drawing 2.
[embodiment 2]
Positive active material is CuS, and conductive material is graphene, and binder is polytetrafluoroethylene (PTFE).Three according to
Mass ratio is that the ratio of 80:10:10 is dried to gelling material in 80 degrees Celsius of baking oven after mixing in dehydrated alcohol, so
Gelling material is uniformly applied to afterwards on sizeable collector niobium sheet (thickness 0.01mm), finally in 60 degrees Celsius of baking ovens
Use GF/D diaphragm material package as anode after drying in standing 12 hours or more.The height that cathode uses with a thickness of 0.2mm thickness
Fine aluminium piece is cut into sizeable, is then polished with fine sandpaper and is cleaned in dehydrated alcohol, and ultrasonic vibration is dry
Negative electrode material is used as after dry.It is in molar ratio 1.3:1 in argon gas ring by anhydrous aluminum chloride and 1- ethyl-3-methylimidazole chloride
It is configured to ionic liquid in the glove box in border, as aluminium ion secondary cell electrolyte of the invention.Finally by it is ready just
Pole piece, negative electrode tab and electrolyte are assembled into Soft Roll aluminium ion battery in glove box.After battery installs 24 hours, in 0.1-2.0V
Between carry out charge-discharge test.
[embodiment 3]
Positive active material is CuS, and conductive material is platinum slurry, and the two is according to the ratio that mass ratio is 80:20 in anhydrous second
It is dried to gelling material in alcohol in 80 degrees Celsius of baking oven after mixing, then gelling material is uniformly applied to size conjunction
In suitable collector niobium sheet (thickness 0.01mm), GF/D diaphragm finally is used after the drying that stands 12 hours or more of 80 degrees Celsius of baking ovens
Material package is used as anode.High-purity aluminium flake that cathode uses with a thickness of 0.2mm thickness, is cut into sizeable,
Then it is polished with fine sandpaper and is cleaned in dehydrated alcohol, and be used as negative electrode material after ultrasonic vibration drying.By anhydrous aluminum chloride
In molar ratio it is that 1.3:1 is configured to ionic liquid in the glove box of ar gas environment with 1- ethyl-3-methylimidazole chloride, makees
For aluminium ion secondary cell electrolyte of the invention.Finally by ready positive plate, negative electrode tab and electrolyte in glove box
It is assembled into Soft Roll aluminium ion battery.After battery installs 24 hours, charge-discharge test is carried out between 0.1-2.0V.
[embodiment 4]
Positive active material is CuS, and conductive material is silver paste, and the two is according to the ratio that mass ratio is 90:10 in anhydrous second
It is dried to gelling material in alcohol in 80 degrees Celsius of baking oven after mixing, then gelling material is uniformly applied to size conjunction
In suitable collector niobium sheet (thickness 0.01mm), GF/D diaphragm finally is used after the drying that stands 12 hours or more of 80 degrees Celsius of baking ovens
Material package is used as anode.High-purity aluminium flake that cathode uses with a thickness of 0.2mm thickness, is cut into sizeable,
Then it is polished with fine sandpaper and is cleaned in dehydrated alcohol, and be used as negative electrode material after ultrasonic vibration drying.By anhydrous aluminum chloride
In molar ratio it is that 1.3:1 is configured to ionic liquid in the glove box of ar gas environment with 1- ethyl-3-methylimidazole chloride, makees
For aluminium ion secondary cell electrolyte of the invention.Finally by ready positive plate, negative electrode tab and electrolyte in glove box
It is assembled into Soft Roll aluminium ion battery.After battery installs 24 hours, charge-discharge test is carried out between 0.1-2.0V.
Claims (5)
1. a kind of CuS is the aluminium ion secondary cell of anode, which includes anode, battery cathode, contains
Aluminium ion nonaqueous solution electrolysis liquid, inert metal paillon collector, diaphragm, lead and battery case, which is characterized in that the anode
Material include micron order or nanoscale CuS, conductive material and binder, the mass percent of the CuS is 60-90%, conduction
The mass percent of material is 10-40% and binder mass percent is 0-10%;The conductive material is carbonaceous material or gold
Belong to slurry, the carbonaceous material includes graphene, conductive carbon black or super carbon；The metal paste includes platinum slurry or silver paste；
The binder is the mixture of one or both of Kynoar or polytetrafluoroethylene (PTFE),
The negative electrode material is the conjunction that metallic aluminium of the purity greater than 90% or metallic aluminium and copper, iron, nickel, lead, bismuth, tin or silver are formed
Gold；
It include aluminum halide and ionic liquid, the molar ratio of the aluminum halide and ionic liquid in the liquid of nonaqueous solution electrolysis containing aluminium ion
For 0.4:1-2.4:1.
2. the aluminium ion secondary cell that a kind of CuS according to claim 1 is anode, which is characterized in that the conduction material
When material is graphene, the mass fraction of conductive material is 10-20%, and the mass fraction of CuS is 70-85%, the quality point of binder
Number is 5-10%；When the conductive material is metal paste, the mass fraction of conductive material is 10-40%, and the mass fraction of CuS is
60-90%。
3. the aluminium ion secondary cell that a kind of CuS according to claim 1 is anode, which is characterized in that the ionic liquid
The anion of body includes F-, Cl-, Br-, I-, PF6 -, CN-, SCN-, [N (CF3SO2)]-Or [N (CN)2]-Ion；Cation includes
Imidazoles drone ion, pyridinium ion, pyrroles's drone ion, piperidines drone ion, morpholine drone ion, quaternary ammonium salt ion, quaternary phosphonium salt ion
Or tertiary sulfosalt ion.
4. a kind of method for preparing the aluminium ion secondary cell that CuS as claimed in any one of claims 1-3 is anode, special
Sign is, specifically includes preparation step below:
Step 1: including that micron order or nanoscale CuS, conductive material, binder proportionally weigh uniform mix respectively by raw material
It closes, gelling material is dried in 60-100 degrees Celsius of baking oven, the inert metal collection for being then uniformly applied to gelling material
It on fluid, is made with a thickness of 0.5-2mm sheet composite positive pole, composite positive pole is wrapped up with diaphragm to get anode is arrived
Material；
Step 2: will dry with a thickness of the metal aluminum or aluminum alloy of 0.1-1mm after fine sandpaper polishing cleaning to get cathode is arrived
Material；
Step 3: aluminum halide and ionic liquid are mixed in the glove box of ar gas environment with molar ratio for 0.4:1-2.4:1, it is quiet
It sets 24 hours or more, that is, is configured to containing the liquid of nonaqueous solution electrolysis containing aluminium ion that can move freely；
Step 4: finally by positive electrode and step 2 that step 1 obtains obtain negative electrode material and step 3 obtain it is non-containing aluminium ion
Aqueous solution electrolysis liquid assembles in glove box, obtains Soft Roll aluminium ion battery or tubular battery, i.e. CuS is the aluminium ion of anode
Secondary cell；
Step 5: after battery pack installs, carrying out charge-discharge test again after liquid whole wetting electrode piece to be electrolysed.
5. the preparation method that CuS according to claim 4 is the aluminium ion secondary cell of anode, which is characterized in that step 1
In, the diaphragm is one of MIcroporous polyolefin film diaphragm material or glass fiber material；The inert metal collector packet
Include tantalum piece, niobium sheet, molybdenum sheet, titanium sheet, nickel foam or gold and platinum group metal.
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| CN107086322B (en) * | 2017-05-03 | 2019-06-07 | 厦门大学 | A kind of copper selenium compound be anode can charge and discharge aluminium ion battery |
| CN107275615A (en) * | 2017-06-29 | 2017-10-20 | 厦门大学 | A kind of sulphur copper compound C-base composte material is the aluminium ion battery of positive pole |
| CN107293693B (en) * | 2017-08-18 | 2019-08-13 | 北京理工大学 | Positive electrode and preparation method thereof for aluminium-sulfur battery |
| CN112678870A (en) * | 2020-12-28 | 2021-04-20 | 北京理工大学 | Aluminum secondary battery and aluminum storage active material thereof |
| CN113725419B (en) * | 2021-09-02 | 2022-09-02 | 吉林大学 | Al-Cu eutectic alloy electrode with lamellar structure, preparation method thereof and application thereof in water-based secondary aluminum ion battery |
| CN114204138B (en) * | 2021-12-15 | 2023-10-20 | 北京化工大学 | Water-based aluminum-ion-containing battery and preparation method thereof |
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