CN109279663A - A kind of borate family anode material of lithium-ion battery and its preparation and application - Google Patents
A kind of borate family anode material of lithium-ion battery and its preparation and application Download PDFInfo
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- CN109279663A CN109279663A CN201811331109.8A CN201811331109A CN109279663A CN 109279663 A CN109279663 A CN 109279663A CN 201811331109 A CN201811331109 A CN 201811331109A CN 109279663 A CN109279663 A CN 109279663A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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 present invention relates to a kind of borate family anode material of lithium-ion battery and its preparation and application, when prepared by material: nickel source, cobalt source and boron source being uniformly mixed, the sintered heat insulating under oxidizing atmosphere with molar ratio 2:1:2~3, obtain purpose product CoNi after cooling2(BO3)2.Compared with prior art, CoNi of the invention2(BO3)2Material, raw material sources are extensive, it is low in cost, have a safety feature and environmental-friendly, the features such as preparation method has process flow simple, and equipment requirement is low, and product purity is high, CoNi obtained2(BO3)2Material shows excellent chemical property.
Description
Technical field
The invention belongs to anode material of lithium-ion battery technical fields, are related to a kind of borate family sodium-ion battery cathode material
Material and its preparation and application.
Background technique
It is cheap, high that ever-increasing renewable energy (wind energy, solar energy, tide energy etc.) promotes researchers constantly to explore
The energy-storage system of effect.The features such as resourceful, low in cost due to sodium, so that sodium-ion battery technology stores large-scale electric energy
There is certain attraction with conversion, can be used as one of alternative of lithium ion battery.Since sodium ion radius is much larger than lithium
Ionic radius, so that traditional lithium ion battery negative material storage sodium performance is poor.Therefore, research and probe height ratio capacity, length are followed
Ring service life and powerful negative electrode material become the key for developing sodium-ion battery.
In the cathode storage sodium material being currently known, graphite material is larger due to sodium ion radius, it is difficult in graphite linings
Deintercalation reaction is carried out, anode material of lithium-ion battery is not suitable for.Hard carbon material is also reported negative applied to sodium-ion battery
Pole material, the results showed that there is preferable storage sodium performance, specific capacity is up to 200-300mAhg-1(Advanced
Functional Materials, 2011,21 (20): 3859-3867).Metal and alloy type negative material are because it is with high
Specific capacity and be concerned by people, the western seminar of Yang Han is designed using nanosizing and gradient-structure, is prepared using ball-milling method
SiC-Sb-Cu-C Core-shell structure material, kernel are SiC material, prepare one layer of Sb/Cu material in SiC core surface to mention
High conductivity, finally outer core surface adds carbon coating layer again.The core-shell material of preparation shows excellent cyclical stability, and 100
Specific capacity maintains 595mAhg after circle circulation-1(Electrochimica Acta, 2013,87,41-45).But such material,
During charge and discharge cycles, the defects of it is low that there are first charge discharge efficiencies, and cubical expansivity is big, and cycle life is undesirable.
When polyanionic boronic acid compound salt is as anode material of lithium-ion battery, there is theoretical specific capacity height, reserves
Abundant, the advantages that environmental-friendly and resource distribution is wide.Yang etc. uses hydro-thermal method, prepares Zn3B2O6, and as sodium ion electricity
Pond negative electrode material, result of study discovery, specific capacity is up to after this composite material recycles 100 times in sodium-ion battery
283.7mAh g-1, and show excellent high rate performance (Bulletin of the Chemical Society of Japan,
2018.).It deepens continuously with people to sodium-ion battery energy storage exploration, researcher, which thirsts for exploitation, has height ratio capacity, excellent
The excellent electrochemical performances such as different high rate performance and the simple new material of preparation method, to meet the development of sodium-ion battery energy storage
Demand.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of borate family sodium from
Sub- cell negative electrode material and its preparation.
The purpose of the present invention can be achieved through the following technical solutions:
It is an object of the present invention to proposing a kind of borate family anode material of lithium-ion battery, chemical formula is
CoNi2(BO3)2。
Further, it is rhombic system, belongs to Pnmn space group.Crystal structure is kotoite type.
The second object of the present invention is the provision of a kind of preparation method of borate family anode material of lithium-ion battery, will
Nickel source, cobalt source and boron source are uniformly mixed with molar ratio 2:1:2~3, the sintered heat insulating under oxidizing atmosphere, obtain mesh after cooling
Product pure phase CoNi2(BO3)2。
Further, the molar ratio of nickel source, cobalt source and boron source is 2:1:2~2.5.It is mixed using dry grinding or wet grinding
Close 2~4h；Then it is sintered in air.If nickel source, cobalt source in the limited range of the present invention, cannot not form pure phase
Purpose product；If boron source content is too low, pure phase purpose product cannot be formed；If boron source too high levels, cause raw material
Waste and the removal of excessive boron are difficult.
Further, oxidizing atmosphere is under air or oxygen atmosphere.Preferably carry out in air atmosphere.
Further, sintering temperature is 800-1200 DEG C, time 1-60h.Further, sintering temperature 800-
1100 DEG C, time 20-60h.Sintering temperature wants moderate, if temperature is too low, pure phase Co cannot be made2Ni(BO3)2Material, if
Temperature is excessively high, then the Co that may be prepared2Ni(BO3)2Material granule increases, and is unfavorable for ion transmission and infiltrates with electrolyte, reduces it
Chemical property.
Further, in sintering process, heating rate control is 1-20 DEG C/min.
Further, the nickel source is any one in nickel oxide, nickel oxalate, nickel nitrate, nickel chloride or nickel sulfate
Kind or several combinations；
The cobalt source be cobaltosic oxide, cobalt oxalate, cobalt nitrate, cobaltous sulfate or cobalt oxide in any one or
Several combinations；
The boron source in diboron trioxide, boric acid, boron nitride, boric acid ammonia or phenyl boric acid any one or it is several
The combination of kind.
The third object of the present invention is the provision of a kind of borate family anode material of lithium-ion battery in sodium-ion battery
In application, wherein sodium-ion battery is formed by working electrode, to electrode, electrolyte and diaphragm, and working electrode material is
CoNi2(BO3)2。
Compared with prior art, CoNi of the invention2(BO3)2Material has preparation process flow simple, to the property of equipment
It can require low, the features such as product purity is high.CoNi obtained2(BO3)2Material has high specific capacity and high rate performance, is a kind of
Anode material of lithium-ion battery with application potential.
Detailed description of the invention
Fig. 1 is the CoNi that embodiment 1 and comparative example 1 are prepared2(BO3)2The XRD spectrum of material；
Fig. 2 is the CoNi that embodiment 1 is prepared2(BO3)21st time, the 2nd time and the 3rd time charging and discharging curve figure of material；
Fig. 3 is the CoNi that embodiment 1 is prepared2(BO3)2Cycle performance figure of the material under 200mA/g current density.
Fig. 4 is the CoNi that embodiment 1 is prepared2(BO3)2High rate performance figure of the material under different electric current densities.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.The present embodiment is with technical solution of the present invention
Premised on implemented, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to
Following embodiments.
The CoNi that the method for the present invention is synthesized2(BO3)2Negative electrode material, conductive carbon black and binder carboxymethyl cellulose
(CMC) 80:10:10 in mass ratio is uniformly mixed, and is coated on copper foil, strikes out negative electrode tab after dry, for 24 hours in 80 DEG C of dryings.
It is to cathode with metallic sodium；Mass ratio is dissolved in 1mol/L for ethylene carbonate (EC)/dimethyl carbonate of 1:1
(DMC) NaClO in mixed solution4Salting liquid is as electrolyte；Button cell is assembled into argon gas glove box.
Electrochemical property test is carried out using the blue electricity CT2001A type cell tester in Wuhan, charging/discharging voltage range is
0.01V~3.0V (vs.Na+/Na).Test temperature is 25 DEG C.
Nickel nitrate and cobalt nitrate in following embodiment are hexahydrate salt.
Embodiment 1
The nickel nitrate of about 3g, the cobalt nitrate of about 1.5g and about 0.7g boric acid is uniform by ground and mixed, in air atmosphere
Under the conditions of be warming up to after 900 DEG C and constant temperature keeps 48h in tube furnace with 5 DEG C/min rate, cooled to room temperature is produced
Object CoNi2(BO3)2Material.
Comparative example 1
The nickel nitrate of about 3g, the cobalt nitrate of about 1.5g and about 0.7g boric acid is uniform by ground and mixed, in air atmosphere
Under the conditions of be warming up to after 750 DEG C and constant temperature keeps 48h in tube furnace with 5 DEG C/min rate, cooled to room temperature is produced
Object CoNi2(BO3)2Material.
By XRD spectrum (Fig. 1) it is found that the CoNi prepared by embodiment 12(BO3)2Material, the CoNi reported with document2
(BO3)2Structure match, illustrate be made material ingredient be pure phase CoNi2(BO3)2.And by comparative example 1,750 DEG C of conditions
Lower obtained product of calcining has Co3BO5Equal impurity, cannot then not synthesize pure phase CoNi in this experimental temperature range2(BO3)2.Figure
2 be CoNi2(BO3)21st time, the 2nd time and the 3rd time charging and discharging curve figure of material, as shown, the charge and discharge of 0.01~3.0V
In voltage range, in first time discharge process, there is an apparent discharge platform, and does not occur in second of discharge process
Identical platform illustrates that material structure change occurs during first charge-discharge, in subsequent charge and discharge process, charge and discharge
Curve essentially coincides, and illustrates that subsequent loop structure maintains stabilization, is conducive to the cycle life kept.Fig. 3 is CoNi2
(BO3)2Cycle performance figure of the material under 200mA/g charging and discharging currents density, as shown, the 2nd discharge capacity is
461.3mA/g, 30 times circulation after CoNi2(BO3)2Capacity still keep 368.2mA/g.Fig. 4 is material high rate performance figure, by scheming
It is found that when discharge current density is 200mA/g, 500mA/g, 1000mA/g, 2000mA/g, two nickel ortho-borate cathode of cobalt
Capacity is respectively 459.1mAh/g, 321.7mAh/g, 271.5mAh/g, 222.5mAh/g.Illustrate to invent the material for sodium from
Sub- battery has excellent high rate performance.
Embodiment 2
The nickel nitrate of about 5.8g, the cobalt nitrate of about 2.9g and about 1.24g boric acid is uniform by ground and mixed, in air gas
After being warming up to 1000 DEG C and constant temperature holding 55h in tube furnace under the conditions of atmosphere with 1 DEG C/min rate, cooled to room temperature is obtained
The product CoNi of pure phase free from admixture2(BO3)2Material.
Embodiment 3
The nickel nitrate of about 6g, the cobalt nitrate of about 3g and about 1.4g boric acid is uniform by ground and mixed, in oxygen atmosphere item
After being warming up to 900 DEG C and constant temperature holding 48h in tube furnace under part with 3 DEG C/min rate, cooled to room temperature obtains pure phase
The product CoNi of free from admixture2(BO3)2Material.
Embodiment 4
The nickel nitrate of about 3g, the cobalt nitrate of about 1.5g and about 0.7g boric acid is uniform by ground and mixed, in air atmosphere
Under the conditions of be warming up to after 1100 DEG C and constant temperature keeps 48h in tube furnace with 3 DEG C/min rate, cooled to room temperature obtains pure
The product CoNi of phase free from admixture2(BO3)2Material.
Embodiment 5
The nickel nitrate of about 3g, the cobalt nitrate of about 1.5g and about 0.7g boric acid is uniform by ground and mixed, in air atmosphere
Under the conditions of be warming up to after 1200 DEG C and constant temperature keeps 55h in tube furnace with 5 DEG C/min rate, cooled to room temperature obtains pure
The product CoNi of phase free from admixture2(BO3)2Material.
Embodiment 6
The nickel nitrate of about 5.8g, the cobalt nitrate of about 2.9g and about 1.24g boric acid is uniform by ground and mixed, in air gas
After being warming up to 1200 DEG C and constant temperature holding 48h in tube furnace under the conditions of atmosphere with 3 DEG C/min rate, cooled to room temperature is obtained
The product CoNi of pure phase free from admixture2(BO3)2Material.
Embodiment 7
Nickel oxide, cobaltosic oxide and diboron trioxide are taken, guarantee nickel: cobalt: the molar ratio of boron is 2:1:2, ground and mixed
Uniformly, the rate in air atmosphere in tube furnace with 1min/ DEG C is warming up to 950 DEG C, and keeps the temperature 60h, after natural cooling i.e.
Obtain the product CoNi of pure phase free from admixture2(BO3)2Material.
Embodiment 8
Nickel oxalate, cobalt oxalate and boron nitride are taken, guarantee nickel: cobalt: the molar ratio of boron is 2:1:3, and ground and mixed is uniform, in sky
Rate under gas atmosphere in tube furnace with 20min/ DEG C is warming up to 1200 DEG C, and keeps the temperature 1h, and pure phase is obtained after natural cooling
The product CoNi of free from admixture2(BO3)2Material.
Embodiment 9
Nickel chloride, cobaltous sulfate and boric acid ammonia are taken, guarantee nickel: cobalt: the molar ratio of boron is 2:1:2.5, and ground and mixed is uniform,
Rate under air atmosphere in tube furnace with 10min/ DEG C is warming up to 1100 DEG C, and keeps the temperature 20h, obtains after natural cooling pure
The product CoNi of phase free from admixture2(BO3)2Material.
Embodiment 10
Nickel sulfate, cobalt oxide and phenyl boric acid are taken, guarantee nickel: cobalt: the molar ratio of boron is 2:1:2.8, and ground and mixed is uniform,
Rate under air atmosphere in tube furnace with 10min/ DEG C is warming up to 800 DEG C, and keeps the temperature 48h, obtains after natural cooling pure
The product CoNi of phase free from admixture2(BO3)2Material.
Embodiment 11
Take mixture (the two quality of nickel sulfate and nickel nitrate mixture (the two mass ratio 1:1), cobalt nitrate and cobaltous sulfate
Than the mixture (the two mass ratio is 1:1) for 1:1), diboron trioxide and boron nitride, guarantee nickel: cobalt: the molar ratio of boron is 2:
1:2.8, ground and mixed is uniform, and the rate in tube furnace with 10min/ DEG C is warming up to 900 DEG C in air atmosphere, and keeps the temperature
40h obtains the product CoNi of pure phase free from admixture after natural cooling2(BO3)2Material.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (9)
1. a kind of borate family anode material of lithium-ion battery, which is characterized in that its chemical formula is CoNi2(BO3)2。
2. a kind of borate family anode material of lithium-ion battery according to claim 1, which is characterized in that it is orthorhombic
System, belongs to Pnmn space group.
3. the preparation method of borate family anode material of lithium-ion battery as claimed in claim 1 or 2, which is characterized in that will
Nickel source, cobalt source and boron source are uniformly mixed with molar ratio 2:1:2~3, the sintered heat insulating under oxidizing atmosphere, obtain mesh after cooling
Product.
4. the preparation method of borate family anode material of lithium-ion battery according to claim 3, which is characterized in that oxidation
Property atmosphere be under air or oxygen atmosphere.
5. the preparation method of borate family anode material of lithium-ion battery according to claim 3, which is characterized in that sintering
Temperature is 800-1200 DEG C, time 1-60h.
6. the preparation method of borate family anode material of lithium-ion battery according to claim 5, which is characterized in that sintering
Temperature is 800-1100 DEG C, time 20-60h.
7. the preparation method of borate family anode material of lithium-ion battery according to claim 3, which is characterized in that sintering
In the process, heating rate control is 1-20 DEG C/min.
8. the preparation method of borate family anode material of lithium-ion battery according to claim 3, which is characterized in that described
Nickel source be any one or several combinations in nickel oxide, nickel oxalate, nickel nitrate, nickel chloride or nickel sulfate；
The cobalt source be cobaltosic oxide, cobalt oxalate, cobalt nitrate, cobaltous sulfate or cobalt oxide in any one or it is several
Combination；
The boron source in diboron trioxide, boric acid, boron nitride, boric acid ammonia or phenyl boric acid any one or it is several
Combination.
9. application of the borate family anode material of lithium-ion battery as claimed in claim 1 or 2 in sodium-ion battery,
In, sodium-ion battery is formed by working electrode, to electrode, electrolyte and diaphragm, working electrode material CoNi2(BO3)2。
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111029570A (en) * | 2019-11-27 | 2020-04-17 | 长沙理工大学 | Cobalt borate/graphene composite material for lithium ion battery cathode and preparation method thereof |
| CN111244444A (en) * | 2020-01-15 | 2020-06-05 | 上海电力大学 | Borate lithium ion battery cathode material and preparation method thereof |
| CN111422880A (en) * | 2020-03-31 | 2020-07-17 | 上海电力大学 | Novel negative electrode material of sodium ion battery and preparation and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106997951A (en) * | 2017-05-15 | 2017-08-01 | 上海电力学院 | It is a kind of for the negative material of sodium-ion battery and its preparation and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106997951A (en) * | 2017-05-15 | 2017-08-01 | 上海电力学院 | It is a kind of for the negative material of sodium-ion battery and its preparation and application |
Non-Patent Citations (1)
| Title |
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| H. GÜLER ET AL.: ""Synthesis and Crystal Structure CoNi2(BO3)2"", 《INORGANIC MATERIALS》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111029570A (en) * | 2019-11-27 | 2020-04-17 | 长沙理工大学 | Cobalt borate/graphene composite material for lithium ion battery cathode and preparation method thereof |
| CN111029570B (en) * | 2019-11-27 | 2023-07-21 | 长沙理工大学 | Cobalt borate/graphene composite material for lithium ion battery cathode and preparation method thereof |
| CN111244444A (en) * | 2020-01-15 | 2020-06-05 | 上海电力大学 | Borate lithium ion battery cathode material and preparation method thereof |
| CN111422880A (en) * | 2020-03-31 | 2020-07-17 | 上海电力大学 | Novel negative electrode material of sodium ion battery and preparation and application thereof |
| CN111422880B (en) * | 2020-03-31 | 2023-04-14 | 上海电力大学 | Negative electrode material of sodium ion battery and preparation and application thereof |
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