CN104091920A - Carbon-coated nano-scale lithium-aluminum alloy negative electrode material and preparation method thereof - Google Patents
Carbon-coated nano-scale lithium-aluminum alloy negative electrode material and preparation method thereof Download PDFInfo
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- CN104091920A CN104091920A CN201410339612.3A CN201410339612A CN104091920A CN 104091920 A CN104091920 A CN 104091920A CN 201410339612 A CN201410339612 A CN 201410339612A CN 104091920 A CN104091920 A CN 104091920A
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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
- H01M4/364—Composites as mixtures
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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
- H01M4/13—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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- 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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/381—Alkaline or alkaline earth metals elements
- H01M4/382—Lithium
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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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 invention discloses a carbon-coated nano-scale lithium-aluminum alloy negative electrode material and a preparation method thereof. The body of the electrode material is lithium-aluminum alloy nanoparticles; the lithium-aluminum alloy nanoparticles are uniformly coated with an organic carbon source by a high temperature solid state method to form an embedded structure, and finally, the carbon-coated lithium-aluminum alloy nanoparticles are obtained through high-temperature calcination and carbonization in an inert atmosphere; the composite material can buffer the volume expansion to prevent collapse of the electrode structure, and meanwhile, good electrical conductivity of the whole electrode can be guaranteed. By adopting the composite material as the lithium ion battery negative electrode material, a lithium ion battery negative electrode material with high lithium storage capacity and good cycle performance can be obtained.
Description
Technical field
The invention belongs to technical field of electrochemistry, be specifically related to a kind of carbon-coated nano level lithium-aluminium alloy negative material and preparation method thereof.
Background technology
Along with economic development, the mankind are increasing to the demand of natural resources, thereby cause the problem such as depletion of natural resources and environmental pollution.So the technology that taps a new source of energy is extremely urgent.Lithium ion battery, as a kind of newer secondary energy sources, has the advantages such as quality is light, operating voltage is high, actual charging and discharging capacity large, environmental protection, is widely applied in the mankind's life, such as mobile phone, notebook computer etc.But along with scientific and technical development, people have higher requirement to the lithium ion battery of industrialization at present, wish that it has higher energy density and power density.
The method of preparing lithium-aluminium alloy has a lot, such as high-energy ball milling method, vacuum melting method, powder metallurgic method, ionic liquid electrodeposition.The coated method of carbon comprises high temperature solid-state method, arc discharge method, liquid impregnation method, pyrolysismethod, chemical vapour deposition technique.Arc discharge method is under inert atmosphere, evaporates graphite electrode just can in the product being deposited in negative electrode or reaction chamber wall, obtain with direct-current arc electric discharge.Chemical vapour deposition (CVD) is in reative cell, and uniform particles that be coated is disperseed, on substrate, to pass at a certain temperature carbon source gas, issues raw pyrolytic reaction and on substrate, is deposited as carbon in the catalytic action of metallic particles.Liquid impregnation method is first to flood ungraphitised carbon with intending coated metal salt solution, then carries out after filtration drying, further in inert atmosphere, carries out high-temperature heat treatment, comprises many Carbon-encapsulated Metal Nanoparticles in product.Pyrolysismethod is using organic genus compound, organometallic polymer or the high-molecular complex etc. that surely exist in air and have a solubility as source metal and suitable carbon source is carried out pyrolysis and can obtain nano metal particles and be dispersed in the composite material of carbon base body in inert atmosphere.High temperature solid-state rule is at high temperature, between solid interface, through contact, reacts, and nucleation, crystal growth response obtains product.
The negative material of present lithium ion battery is mainly material with carbon element, comprises graphitized carbon material, as graphitized intermediate-phase carbosphere and some pyrolyzed hard carbons.At present, its actual specific capacity is generally no more than 400mAh/g, cannot meet the needs of real new-energy automobile and high-end electronic devices.
Lithium metal has the most negative current potential and the highest specific discharge capacity (3860mAh/g), but in charge and discharge process, has dendrite and intrinsic safety problem.Lithium and aluminium form AlLi alloy, and specific discharge capacity, up to 993mAh/g, can have been avoided the generation of dendrite, simultaneously voltage ratio graphite wants high, but it in charge and discharge process, change in volume is very large, cause the variation of material structure, the decay of capacity and the deterioration of cycle performance.
Summary of the invention
For the deficiencies in the prior art, technical problem to be solved by this invention is to provide a kind of lithium ion battery carbon-coated nano level lithium-aluminium alloy negative material and preparation method thereof, this material lithium storage content is high, good cycle, preparation method is simple, cost is low, the electrode material of the carbon-coated nano level lithium-aluminium alloy that the present invention proposes, it is not simply mixed and forms with alloy particle by material with carbon element, but by organic carbon source carbon and bulk material embedded type structure that evenly coated at high temperature carburizing reagent of alloy particle forms, its carbon-coating is combined closely with the alloy material of body, be difficult for peeling off, and there are certain expansibility and contractibility and good electron conduction ability.
The concrete technical scheme of the present invention is to provide a kind of carbon-coated nano level lithium-aluminium alloy negative material and preparation method thereof, and preparation method specifically comprises the following steps: the lithium sheet that is 1) 1:1 ~ 3:1 by ratio and aluminium powder and 3 ~ 5g are dry, and sodium chloride is prepared lithium-aluminium alloy nano particle through high-energy ball milling method under inert atmosphere;
2) add the abundant ball milling of organic carbon source, it is mixed;
3) by high temperature solid-state method, by the material after the ball milling mixing, under inert atmosphere, after high-temperature calcination carbonization, obtain carbon-coated nano level lithium-aluminium alloy negative material.
High-energy ball milling method described in step 1) is prepared the Ball-milling Time 10-15h of lithium-aluminium alloy powder.
The lithium-aluminium alloy diameter of particle of described high-energy ball milling method gained is at nanoscale.
Described high-energy ball milling utilizes the rotation and vibration of ball mill to make hard sphere carry out strong shock to raw material, grind and stir, metal or alloy powder is pulverized to the method for nanometer particle, compared with other physical methods, this method is simple and practical, can under comparatively gentle condition, prepare nano level metal alloy, and its Tissue distribution is even.
Step 2) described organic carbon source is any in citric acid, ascorbic acid, glucose, NMP, pitch, phenolic resins.
Described in step 3), high temperature solid-state method specifically refers to step 2) the ball milling mixing after material be positioned in the inert gas of tube furnace, in a certain temperature range, heat-treat.
Inert atmosphere described in step 3) is any in argon gas, helium.
Described in step 3), high-temperature calcination temperature range is 500-700 DEG C, and temperature retention time is 1 ~ 6 hour, and in the coated lithium-aluminium alloy nano particle of carbon finally obtaining, the content of carbon accounts for 10 1 30wt% of composite material gross mass.
A kind of carbon-coated nano level lithium-aluminium alloy negative material that described preparation method prepares.
The body of described material is lithium-aluminium alloy particle, and carbon coating layer is to be evenly intactly coated on alloy nanoparticle sub-surface, and its carbon content accounts for 10% one 30% of composite material gross mass.
If carbon content is less than 10%, because carbon content is too low, cannot make lithium-aluminium alloy particle disperse completely, if carbon content is greater than 30%, because the capacity of this part material with carbon element itself is lower, thereby reduce to a great extent the capacity of whole composite material.
The invention has the beneficial effects as follows: in carbon-coated nano level lithium-aluminium alloy negative material of the present invention, the distribution of carbon is embedded type.In the structure of this composite material, lithium-aluminium alloy nano particle is evenly dispersed in carbon dispersible carrier, form uniform two-phase composites, in charge and discharge process, lithium-aluminium alloy nano particle is the activated centre of electrochemical reaction, although carbon carrier has the ability of removal lithium embedded, mainly play transmission channel and the supporter effect of ion, electronics.Therefore,, in cyclic process, this composite material can buffer volumes expand, and prevents that electrode structure from caving in, and has ensured the good electric conductivity of overall electrode simultaneously.Adopt this composite material can obtain as lithium ion battery negative material the lithium ion battery negative material that lithium storage content is high, cycle performance is good, adopt carbon-coated nano level lithium-aluminium alloy combination electrode material of the present invention, can be used for lithium ion battery negative, it is embedded type structure, its specific capacity is bright higher than traditional graphite cathode material, and cycle performance is also better than common alloy material greatly.
Brief description of the drawings
Fig. 1 is the coated illustraton of model of the carbon of embedded type.
In figure: 1, carbon 2, lithium-aluminium alloy nano particle.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further details, but is not limitation of the present invention.
Embodiment 1
Lithium sheet and aluminium powder are put into ball grinder in the ratio of certain 2.8:1 to be mixed, get the stainless steel ball that several vary in size, ball and raw material are put into ball grinder in the lump, then gas in ball grinder is found time, and be filled with argon shield, add the dry salt of 1g to make grinding aid, prevent that powder from luming in mechanical milling process, obtain a certain amount of lithium-aluminium alloy powder. get the lithium-aluminium alloy powder 10.0g of above-mentioned preparation, get the lithium-aluminium alloy powder 10g preparing, add again the glucose of 3g, fully ball milling, be placed in 650 DEG C of calcinings of tube furnace 3 hours, obtain carbon-coated nano level lithium-aluminium alloy electrode material.
Embodiment 2
Lithium sheet and aluminium powder are put into ball grinder in the ratio of certain 1.5:1 to be mixed; get the stainless steel ball that several vary in size; ball and raw material are put into ball grinder in the lump; then gas in ball grinder is found time; and be filled with argon shield; the dry salt that adds 1g is made grinding aid; prevent that powder from luming in mechanical milling process; obtain a certain amount of lithium-aluminium alloy powder. get the lithium-aluminium alloy powder 10.0g of above-mentioned preparation; add 1.5g porous charcoal; fully ball milling, obtains carbon-coated nano level lithium-aluminium alloy electrode material.
Embodiment 3
The ratio of lithium sheet and aluminium powder 1.2:1 is put into ball grinder to be mixed; get the stainless steel ball that several vary in size; ball and raw material are put into ball grinder in the lump; then gas in ball grinder is found time; and be filled with argon shield; add the salt that 1g is dry to make grinding aid, prevent that powder from luming in mechanical milling process.Get the pitch of 4.0g, be dissolved in the carbon disulfide of certain volume, stir until its dissolving, add again the lithium-aluminium alloy powder of 10.0g, isolate presoma, under argon gas atmosphere, dry, be placed in 700 DEG C of calcinings of tube furnace 4 hours, obtain carbon-coated nano level lithium-aluminium alloy electrode material.
Claims (9)
1. a preparation method for carbon-coated nano level lithium-aluminium alloy negative material, is characterized in that specifically comprising the following steps: the lithium sheet that is 1) 1:1 ~ 3:1 by ratio and aluminium powder and 1 ~ 5g are dry, and sodium chloride is prepared lithium-aluminium alloy nano particle through high-energy ball milling method under inert atmosphere;
2) add the abundant ball milling of organic carbon source, it is mixed;
3) by high temperature solid-state method, by the material after the ball milling mixing, under inert atmosphere, after high-temperature calcination carbonization, obtain carbon-coated nano level lithium-aluminium alloy negative material.
2. according to the preparation method described in claim 1, it is characterized in that the high-energy ball milling method described in step 1) prepares the Ball-milling Time 10-15h of lithium-aluminium alloy powder.
3. preparation method according to claim 2, is characterized in that the lithium-aluminium alloy diameter of particle of described high-energy ball milling method gained is at nanoscale.
4. according to the preparation method described in claim 1, it is characterized in that step 2) described organic carbon source is any in citric acid, ascorbic acid, glucose, NMP, pitch, phenolic resins.
5. according to the preparation method described in claim 1, it is characterized in that described in step 3) that high temperature solid-state method specifically refers to step 2) the ball milling mixing after material be positioned in the inert gas of tube furnace, in a certain temperature range, heat-treat.
6. according to the preparation method described in claim 1, it is characterized in that inert atmosphere described in step 3) is any in argon gas, helium.
7. according to the preparation method described in claim 1, it is characterized in that described in step 3) that high-temperature calcination temperature range is 500-700 DEG C, temperature retention time is 1 ~ 6 hour, and in the coated lithium-aluminium alloy nano particle of carbon finally obtaining, the content of carbon accounts for 10 1 30wt% of composite material gross mass.
8. a kind of carbon-coated nano level lithium-aluminium alloy negative material of preparing according to preparation method described in claim 1-6.
9. a kind of carbon-coated nano level lithium-aluminium alloy negative material described according to Claim 8, the body that it is characterized in that described material is lithium-aluminium alloy particle, carbon coating layer is to be evenly intactly coated on alloy nanoparticle sub-surface, and its carbon content accounts for 10% one 30% of composite material gross mass.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105680011A (en) * | 2016-01-19 | 2016-06-15 | 天津理工大学 | Preparation method of carbon-coated AlCuFe quasicrystal alloy composite material and application |
| CN107293701A (en) * | 2016-03-31 | 2017-10-24 | 比亚迪股份有限公司 | A kind of lithium ion battery anode active material and preparation method thereof, negative pole and the lithium ion battery comprising the negative pole |
| CN107828374A (en) * | 2017-12-12 | 2018-03-23 | 戚明海 | A kind of novel C MP grinding agents and its manufacture method |
| CN109037606A (en) * | 2018-06-22 | 2018-12-18 | 合肥国轩高科动力能源有限公司 | A kind of carbon coating porous silicon Antaciron composite negative pole material and its preparation, application |
| CN109686944A (en) * | 2018-12-21 | 2019-04-26 | 福建翔丰华新能源材料有限公司 | A kind of carbon coating lithium alloy combination electrode material and preparation method thereof |
| CN111710851A (en) * | 2020-04-27 | 2020-09-25 | 常州赛得能源科技有限公司 | Solid-state battery and preparation method thereof |
| CN112301271A (en) * | 2019-07-26 | 2021-02-02 | 宝山钢铁股份有限公司 | Carbon-oxide electrolyte coated battery negative electrode material and preparation method thereof |
| CN114619025A (en) * | 2020-12-11 | 2022-06-14 | 国家能源投资集团有限责任公司 | Carbon-coated metal nanoparticles and preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105680011A (en) * | 2016-01-19 | 2016-06-15 | 天津理工大学 | Preparation method of carbon-coated AlCuFe quasicrystal alloy composite material and application |
| CN107293701A (en) * | 2016-03-31 | 2017-10-24 | 比亚迪股份有限公司 | A kind of lithium ion battery anode active material and preparation method thereof, negative pole and the lithium ion battery comprising the negative pole |
| CN107828374A (en) * | 2017-12-12 | 2018-03-23 | 戚明海 | A kind of novel C MP grinding agents and its manufacture method |
| CN109037606A (en) * | 2018-06-22 | 2018-12-18 | 合肥国轩高科动力能源有限公司 | A kind of carbon coating porous silicon Antaciron composite negative pole material and its preparation, application |
| CN109686944A (en) * | 2018-12-21 | 2019-04-26 | 福建翔丰华新能源材料有限公司 | A kind of carbon coating lithium alloy combination electrode material and preparation method thereof |
| CN109686944B (en) * | 2018-12-21 | 2022-05-31 | 四川翔丰华新能源材料有限公司 | Carbon-coated lithium alloy composite electrode material and preparation method thereof |
| CN112301271A (en) * | 2019-07-26 | 2021-02-02 | 宝山钢铁股份有限公司 | Carbon-oxide electrolyte coated battery negative electrode material and preparation method thereof |
| CN111710851A (en) * | 2020-04-27 | 2020-09-25 | 常州赛得能源科技有限公司 | Solid-state battery and preparation method thereof |
| CN114619025A (en) * | 2020-12-11 | 2022-06-14 | 国家能源投资集团有限责任公司 | Carbon-coated metal nanoparticles and preparation method and application thereof |
| CN114619025B (en) * | 2020-12-11 | 2023-09-29 | 国家能源投资集团有限责任公司 | Carbon-coated metal nanoparticle, and preparation method and application thereof |
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