CN108321358A - A kind of lithium ion battery negative material and preparation method thereof - Google Patents
A kind of lithium ion battery negative material and preparation method thereof Download PDFInfo
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- CN108321358A CN108321358A CN201710027738.0A CN201710027738A CN108321358A CN 108321358 A CN108321358 A CN 108321358A CN 201710027738 A CN201710027738 A CN 201710027738A CN 108321358 A CN108321358 A CN 108321358A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/134—Electrodes based on metals, Si or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1395—Processes of manufacture of electrodes based on metals, Si or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
Kamash alloy/carbon composite and preparation method thereof that the present invention provides a kind of for lithium ion battery negative material.According to a certain ratio by metal salt and organic ligand, porous, organometallic skeleton material material is prepared in stirring and dissolving, room temperature or solvent thermal reaction in a solvent（Metal organic framework, MOF）, pink salt is added in MOF, is allowed to fully adsorb, the MOF precursor powders containing pink salt are calcined in air and charing obtains a nanometer tin-cobalt alloy/carbon composite in inert gas.Nanometer kamash alloy/carbon composite pattern prepared by the present invention is regular polyhedron ball-type, and nanometer kamash alloy size is less than 10nm, is evenly dispersed in porous polyhedron carbon matrix.When the material is used for negative electrode of lithium ion battery, there is high reversible capacity, good cyclical stability and high rate capability.
Description
Technical field
The present invention relates to lithium ion battery negative materials, more particularly to a kind of alloy/carbon composite, with organic metal
Frame material is the preparation method of template fabricated in situ lithium ion battery nanometer kamash alloy/carbon composite.
Background technology
Lithium ion battery is as current the most widely used secondary cell, with energy density is high, cycle-index is more, nothing
Memory effect, many advantages, such as having a safety feature, is environmental-friendly.And negative material is the key that one of lithium ion battery development.
Extensive use of the graphite negative electrodes material in lithium ion battery at present is based primarily upon its high coulombic efficiency and excellent cycle
Performance.However due to the limitation of itself relatively low lithium storage content（372 mA h g-1, LiC6）, gradually cannot be satisfied quickly
The electric vehicle of development, hybrid vehicle and wind power generation electric energy storage device etc. are to lithium ion cell high-capacity and high-power performance
Requirement.Therefore, develop it is novel there is large capacity, high magnification and the lithium ion battery electrode material of long-life cause
Scientists are greatly paid close attention to.Higher lithium storage content is presented in metal, alloy and metal oxide and lithium ion, it is considered to be pure
One of the alternative materials of graphite negative electrodes material.In the metal and metal oxide negative material of numerous high power capacity, tinbase material
Material is with its higher lithium storage content（ Sn = 991 mA h g-1, SnO2 = 781 mA h g-1, SnS2 = 645 mA h g-1）, lower storage lithium current potential and simple synthetic method and be concerned.However tin class material with lithium ion alloying mistake
Produced enormousness expansion, has thus added up larger stress in material internal, can cause the group of tin-based material structure in journey
It is poly-, it destroys, seriously affects its cyclical stability.To overcome the problems, such as this, widely used method includes：Prepare Sn-M（M=Ni,
Cu, Co）The inactive alloy of isoreactivity-；Prepare tin/carbon composite.It is non-live in cyclic process by taking tin-cobalt alloy as an example
Property the generation of cobalt simple substance there is the active tin of isolation, the effect of rock-steady structure.Meanwhile it if can be inhaled using charcoal as buffer layer
Receive charge and discharge process in volume change, can effectively improve material cyclical stability [Park C M, Kim J H, Kim H,
et al. Chem Soc Rev, 2010, 39 (8): 3115-3141]。
The preparation method of tin alloy includes ball milling [Ferguson P P, Martine M L, Dunlap R A, et
al. Electrochimica Acta, 2009, 54(19):4534-4539], co-precipitation [Zhu J, Wang D, Liu
T, et al. Electrochimica Acta, 2014, 125:347-353] etc..And charcoal cladding typically uses external carbon
Source is realized using high temperature solid-state method.In the process, it is difficult to control size and the dispersion of alloy.Therefore, the present invention carries for the first time
Go out and has utilized Porous transition metal frame material（Metal-organic framework, MOF）As template, while providing gold
Category and carbon source adsorb pink salt using its porous feature, compound using a step high temperature solid-state method fabricated in situ nanometer kamash alloy/charcoal
Material.
Invention content
The purpose of the present invention is to solve the size Control and scattering problem of Sn-containing alloy class negative material, provide one kind
Novel kamash alloy/carbon composite and preparation method thereof.Nanometer kamash alloy prepared by the present invention/carbon composite pattern rule
Whole, tin alloy is uniform to be dispersed in polyhedron carbon matrix.Its specific preparation method includes the following steps：
Step 1：Metal salt and organic ligand are dissolved in solvent；
Step 2：Two kinds of solution in step 1 are mixed, are reacted 1 ~ 24 hour at 0 ~ 200 DEG C.The washing of gained precipitating solvent,
Filtering.It is dried in vacuo at 80 ~ 200 DEG C, obtains MOF；
Step 3：A certain amount of pink salt is dissolved in solvent, is added in step 2 in gained MOF, the mass ratio of pink salt and MOF are
0.5:1 to 5:1；
Step 4：Gained mixture is calcined 1 ~ 6 hour at 150 ~ 250 DEG C in air in step 3；
Step 5：Gained mixture carbonizes 1 ~ 10 hour at 400 ~ 900 DEG C under inert gas shielding in step 4.Obtain target
Product nano kamash alloy/carbon composite.
In step 1, selected salt is metal（Cobalt, iron, nickel, copper, manganese etc.）Nitrate, sulfate, chloride, acetate
Deng.
In step 1, selected organic ligand be imidazoles, 2-methylimidazole, 2- nitroimidazoles, 2,6- naphthalene dicarboxylic acids, to benzene two
Formic acid, 2,5-Dihydroxyterephthalic acid, trimesic acid, 2, one kind or combinations thereof in 2 '-bipyridyls, preferably imidazoles are matched
Body.
In step 1, selected solvent is in methanol, ethyl alcohol, n,N-Dimethylformamide, n,N-dimethylacetamide, acetone
One kind or combinations thereof, preferred methanol.
In step 2, reaction condition is normal stress reaction, or the solvent thermal reaction in sealing water heating kettle.
In step 3, selected pink salt is chloride, sulfate, the acetate etc. of tin.
In step 3, selected solvent is one kind or combinations thereof in water, methanol, ethyl alcohol.
In step 5, selected inert gas is one kind in nitrogen, argon gas.
Compared with existing lithium ion battery kamash alloy material or the preparation method of kamash alloy/carbon composite,
The advantage of the invention is that：Using MOF as template, while metal and carbon source are provided, its characterization of adsorption is recycled to absorb tin source, it is high
Warm solution fabricated in situ, realizes the nanosizing of alloy particle, while ensure that its dispersibility.The common work of inert metal and charcoal
The high rate performance of material, the enhancing of uniform porous layer of charcoal are improved with the alloy of the stability for maintaining material structure, nanosizing
The infiltration of electrolyte and the diffusion of ion, electronics, and then improve the chemical property of material.
The nanometer kamash alloy synthesized to the present invention/carbon composite carries out charge-discharge test（0.01 ~ 3V of voltage range）,
Material shows high specific capacity, good cyclical stability and excellent high rate performance.100 mA g-1It is first under current density
Secondary reversible capacity is 900 mA h g-1Left and right, the capacity retention ratio of 100 cycles is 85% or more.In 2 A g-1High current
Under density, capacity can be stably held in 400 mA h g-1Left and right.
Description of the drawings
Fig. 1 is the stereoscan photograph of nanometer tin-cobalt alloy/carbon composite in the embodiment of the present invention 1.
Fig. 2 is nanometer tin-cobalt alloy/charging and discharging curve of the carbon composite under different current densities in embodiment 1.
Specific implementation mode
With reference to specific embodiment, the present invention is further elaborated, but the present invention is not limited to following embodiments.Institute
It is conventional method to state method unless otherwise instructed.
Embodiment one：
1）1.2g cabaltous nitrate hexahydrates are weighed, is added in 100mL methanol and is evenly stirred until clarification.Take 1.4g ligand 2- methyl miaows
Azoles is dissolved in 100mL methanol, is stirred to clarify.Above two solution is mixed, is reacted at room temperature for 24 hours.Product is centrifuged, is obtained purple
Color precipitates.With ethyl alcohol centrifuge washing 3 times.It is dried in vacuo 8h at 100 DEG C, obtains Co-MOF.
2）It weighs 1g Tin tetrachloride pentahydrates to be dissolved in 500 microlitres of ethyl alcohol, adds to 500mg steps 1）Middle gained Co-MOF
In.By gained mixed solution at 180 DEG C, 4h is calcined in air.
3）By step 2）Under an argon atmosphere, 5 DEG C of every point of heating rates rise to 550 DEG C to gained mixture, keep the temperature 4h.It is cooling
Up to nanometer tin-cobalt alloy/carbon composite.
The whole pattern of gained composite material is as shown in Figure 1.
Using the nanometer tin-cobalt alloy/carbon composite synthesized in embodiment 1 as active material, half-cell performance survey is carried out
Examination.Constant current charge-discharge carries out on blue electric tester.The charge and discharge section of test be 0.01 ~ 3V, current density 100,200,
500、1000、2000 mA h g-1As shown in Fig. 2, showing that the lithium titanate/carbon composite synthesized by this method has
Excellent high rate performance.100 mA g-1Reversible capacity is 945 mA h g for the first time under current density-1, 100 times cycle after capacity
It is maintained at 820 mA h g-1, 2 A g-1Current density under reversible capacity in 475 mA h g-1.
Embodiment two：
1）1.2g cabaltous nitrate hexahydrates are weighed, is added in 100mL methanol and is evenly stirred until clarification.Take 1.4g ligand 2- methyl miaows
Azoles is dissolved in 100mL methanol, is stirred to clarify.Above two solution is mixed, is reacted at room temperature for 24 hours.Product is centrifuged, is obtained purple
Color precipitates.With ethyl alcohol centrifuge washing 3 times.It is dried in vacuo 8h at 100 DEG C, obtains Co-MOF.
2）It weighs 500mg stannous chloride to be dissolved in 500 microlitres of ethyl alcohol, adds to 500mg steps 1）In middle gained Co-MOF.
By gained mixed solution at 180 DEG C, 4h is calcined in air.
3）By step 2）Under an argon atmosphere, 5 DEG C of every point of heating rates rise to 550 DEG C to gained mixture, keep the temperature 4h.It is cooling
Up to nanometer tin-cobalt alloy/carbon composite.
Gained nanometer tin-cobalt alloy/carbon composite is in 100 mA g-1Reversible capacity is 903 mA for the first time under current density
h g-1, 100 times cycle after capacity be maintained at 790mA h g-1, 2 A g-1Current density under reversible capacity in 430 mA h g-1.
Embodiment three：
1）1.2g cabaltous nitrate hexahydrates are weighed, is added in 100mL methanol and is evenly stirred until clarification.Take 1.4g ligand 2- methyl miaows
Azoles is dissolved in 100mL methanol, is stirred to clarify.Above two solution is mixed, is reacted at room temperature for 24 hours.Product is centrifuged, is obtained purple
Color precipitates.With ethyl alcohol centrifuge washing 3 times.It is dried in vacuo 8h at 100 DEG C, obtains Co-MOF.
2）It weighs 500mg stannous chloride to be dissolved in 500 microlitres of ethyl alcohol, adds to 500mg steps 1）In middle gained Co-MOF.
By gained mixed solution at 180 DEG C, 4h is calcined in air.
3）By step 2）Under an argon atmosphere, 5 DEG C of every point of heating rates rise to 700 DEG C to gained mixture, keep the temperature 2h.It is cooling
Up to nanometer tin-cobalt alloy/carbon composite.
Gained nanometer tin-cobalt alloy/carbon composite is in 100 mA g-1Reversible capacity is 930 mA for the first time under current density
h g-1, 100 times cycle after capacity be maintained at 780mA h g-1, 2 A g-1Current density under reversible capacity in 405 mA h g-1.
Example IV：
1）1.2g cabaltous nitrate hexahydrates are weighed, is added in 40mL methanol and is evenly stirred until clarification.Take 1.4g ligand 2,6- naphthalenes two
Carboxylic acid is dissolved in 40mL methanol, is stirred to clarify.Above two solution is mixed, is loaded in 100mL water heating kettles, it is anti-at 120 DEG C
Answer 12h, natural cooling.Product is centrifuged, purple precipitation is obtained.With ethyl alcohol centrifuge washing 3 times.It is dried in vacuo 8h at 100 DEG C, is obtained
Co-MOF。
2）It weighs 500mg stannous chloride to be dissolved in 500 microlitres of ethyl alcohol, adds to 500mg steps 1）In middle gained Co-MOF.
By gained mixed solution at 180 DEG C, 4h is calcined in air.
3）By step 2）Under an argon atmosphere, 5 DEG C of every point of heating rates rise to 550 DEG C to gained mixture, keep the temperature 4h.It is cooling
Up to nanometer tin-cobalt alloy/carbon composite.
Embodiment five：
1）1g cobalt acetates are weighed, is added in 100mL methanol and is evenly stirred until clarification.1g ligand imidazoles is taken to be dissolved in 100mL methanol
In, it stirs to clarify.Above two solution is mixed, is reacted for 24 hours at 80 DEG C.Product is centrifuged, purple precipitation is obtained.With ethyl alcohol from
The heart washs 3 times.It is dried in vacuo 8h at 100 DEG C, obtains Co-MOF.
2）It weighs 500mg stannous chloride to be dissolved in 500 microlitres of ethyl alcohol, adds to 500mg steps 1）In middle gained Co-MOF.
By gained mixed solution at 180 DEG C, 4h is calcined in air.
3）By step 2）Under an argon atmosphere, 5 DEG C of every point of heating rates rise to 550 DEG C to gained mixture, keep the temperature 4h.It is cooling
Up to nanometer tin-cobalt alloy/carbon composite.
Gained nanometer tin-cobalt alloy/carbon composite is in 100 mA g-1Reversible capacity is 850 mA for the first time under current density
h g-1, 100 times cycle after capacity be maintained at 730mA h g-1, 2 A g-1Current density under reversible capacity in 401 mA h g-1.
Embodiment six：
1）1.2g cabaltous nitrate hexahydrates are weighed, is added in 100mL n,N-Dimethylformamide and is evenly stirred until clarification.It takes
1.2g ligand 2- nitroimidazoles are dissolved in 100mL methanol, are stirred to clarify.Above two solution is mixed, is reacted at room temperature
24h.Product is centrifuged, purple precipitation is obtained.With ethyl alcohol centrifuge washing 3 times.It is dried in vacuo 8h at 100 DEG C, obtains Co-MOF.
2）It weighs 500mg butters of tin to be dissolved in 500 microlitres of ethyl alcohol, adds to 500mg steps 1）In middle gained Co-MOF.
By gained mixed solution at 180 DEG C, 4h is calcined in air.
3）By step 2）Under an argon atmosphere, 5 DEG C of every point of heating rates rise to 550 DEG C to gained mixture, keep the temperature 4h.It is cooling
Up to nanometer tin-cobalt alloy/carbon composite.
Embodiment seven：
1）2g Fe(NO3)39H2Os are weighed, is added in 100mL DMF and is evenly stirred until clarification.Take 2.0g ligand terephthalic acid (TPA)s
It is dissolved in 100mL DMF.Above two solution is mixed, loaded in water heating kettle, reacts 12h at 180 DEG C.Product is centrifuged, is used
Ethyl alcohol centrifuge washing 3 times.It is dried in vacuo 8h at 100 DEG C, obtains Fe-MOF.
2）It weighs 500mg stannous chloride to be dissolved in 500 microlitres of ethyl alcohol, adds to 2g steps 1）In middle gained Fe-MOF.By institute
Mixed solution is obtained at 200 DEG C, 2h is calcined in air.
3）By step 2）Under an argon atmosphere, 5 DEG C of every point of heating rates rise to 550 DEG C to gained mixture, keep the temperature 2h.It is cooling
Up to nanometer tin ferroalloy/carbon composite.
Gained nanometer tin ferroalloy/carbon composite is in 100 mA g-1Reversible capacity is 790 mA for the first time under current density
h g-1, 100 times cycle after capacity be maintained at 650mA h g-1, 2 A g-1Current density under reversible capacity in 385 mA h g-1.
Embodiment eight：
1）2g Nickelous nitrate hexahydrates are weighed, 0.5g 2,5-Dihydroxyterephthalic acids are added to 80mL water, ethyl alcohol, DMF volumes
Than being 1:1:In 1 mixed solution, stirring, loaded in water heating kettle, 100 DEG C of reactions are for 24 hours.Product is centrifuged, is washed with ethyl alcohol centrifugation
It washs 3 times.It is dried in vacuo 8h at 100 DEG C, obtains Ni-MOF.
2）It weighs 500mg stannous chloride to be dissolved in 500 microlitres of ethyl alcohol, adds to 2g steps 1）In middle gained Ni-MOF.By institute
Mixed solution is obtained at 200 DEG C, 2h is calcined in air.
3）By step 2）Under an argon atmosphere, 5 DEG C of every point of heating rates rise to 550 DEG C to gained mixture, keep the temperature 2h.It is cooling
Up to nanometer tin-nickel alloy/carbon composite.
Gained nanometer tin-nickel alloy/carbon composite is in 100 mA g-1Reversible capacity is 890 mA for the first time under current density
h g-1, 100 times cycle after capacity be maintained at 700mA h g-1, 2 A g-1Current density under reversible capacity in 435 mA h g-1.
Presently preferred embodiments of the present invention is illustrated above, but the present invention is not limited to the embodiment, is familiar with
Those skilled in the art can also make various equivalent modifications or replacement under the premise of without prejudice to spirit of that invention, these etc.
Same modification or replacement is all contained in the application claim limited range.
Claims (10)
1. a kind of nanometer kamash alloy/carbon composite for lithium ion battery negative material, regular appearance, nanometer tinbase
Alloy size is less than 10nm, and uniform is dispersed in porous polyhedron carbon matrix.
2. the preparation of kamash alloy/carbon composite described in claim 1, it is characterised in that following preparation method：
Step 1：It will be dissolved in solvent together with metal salt and organic ligand；
Step 2：Solution in step 1 is reacted 1 ~ 24 hour at 0 ~ 200 DEG C, gained precipitating solvent washing, filtering, 80 ~
It is dried in vacuo at 200 DEG C, obtains metal-organic framework material（MOF）；
Step 3：A certain amount of pink salt is dissolved in solvent, is added in step 2 in the MOF of gained, the mass ratio of pink salt and MOF
It is 0.5:1 to 5 to 1；
Step 4：Gained mixture is calcined 1 ~ 6 hour at 150 ~ 250 DEG C in air in step 3；
Step 5：Gained mixture carbonizes 1 ~ 10 hour under 400 ~ 900 DEG C, inert gas shielding in step 4, obtains target
Product nano kamash alloy/carbon composite.
3. according to claim 2, the preparation method of a kind of nanometer of kamash alloy/carbon composite, it is characterised in that：It is selected
Salt is the nitrate, sulfate, chloride, acetate etc. of metallic cobalt, iron, nickel, copper, manganese etc..
4. according to claim 2, the preparation method of a kind of nanometer of kamash alloy/carbon composite, it is characterised in that：It is selected
Solvent is one kind or combinations thereof in methanol, ethyl alcohol, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, acetone.
5. according to claim 2, the preparation method of a kind of nanometer of kamash alloy/carbon composite, it is characterised in that：It is selected
Organic ligand is imidazoles, 2-methylimidazole, 2- nitroimidazoles, 2,6 naphthalene dicarboxylic acid, terephthalic acid (TPA), trimesic acid, 2,5-
Dihydric para-phthalic acid, one kind or combinations thereof in 2,2 '-bipyridyls, preferably glyoxaline ligand.
6. according to claim 2, the preparation method of a kind of nanometer of kamash alloy/carbon composite, it is characterised in that：Reaction
Condition is synthesis under normal pressure, or the solvent thermal reaction in sealing water heating kettle.
7. according to claim 2, the preparation method of a kind of nanometer of kamash alloy/carbon composite, it is characterised in that：It is selected
Pink salt is chloride, sulfate, the acetate etc. of tin.
8. according to claim 2, the preparation method of a kind of nanometer of kamash alloy/carbon composite, it is characterised in that：Dissolving
Solvent selected by pink salt is one kind or combinations thereof in water, methanol, ethyl alcohol.
9. according to claim 2, the preparation method of a kind of nanometer of kamash alloy/carbon composite, it is characterised in that：It is preferred that
Carbonization time be 2-4 hours.
10. kamash alloy/carbon composite described in claim 1, when being used as lithium ion battery negative material, 100 mA g-1
Reversible capacity is 900 mA h g for the first time under current density-1Or so, capacity is maintained at 800 mA h g after 100 cycles-1It is left
The right side, and there is good high rate performance, in 2 A g-1Current density under reversible capacity in 400 mA h g-1Left and right.
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