CN103022447B - The preparation method of serondary lithium battery negative pole Sn-Co-C composite material and serondary lithium battery - Google Patents
The preparation method of serondary lithium battery negative pole Sn-Co-C composite material and serondary lithium battery Download PDFInfo
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- CN103022447B CN103022447B CN201210555481.3A CN201210555481A CN103022447B CN 103022447 B CN103022447 B CN 103022447B CN 201210555481 A CN201210555481 A CN 201210555481A CN 103022447 B CN103022447 B CN 103022447B
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention provides a kind of method preparing serondary lithium battery negative pole Sn-Co-C composite material, with the mol ratio of Sn:Co:C for 3:2:1 takes Xi Yuan, cobalt source and carbon source, add appropriate amount of deionized water, general milling 2 ~ 5h, by described mixture calcining at constant temperature 6 ~ 12h at 700 ~ 1100 DEG C in nitrogen atmosphere, naturally after cooling, grinding, obtain Sn-Co-C composite negative pole material, and the serondary lithium battery of the composite material negative pole adopting said method to prepare; By the synthetic method that uses in the present invention and condition, the serondary lithium battery negative pole Sn-Co-C composite material with good cyclicity, higher specific capacity can be prepared easily and fast.
Description
Technical field
The invention belongs to cell art, be specifically related to a kind of preparation method and serondary lithium battery of serondary lithium battery anode material.
Background technology
Secondary cell, is also called rechargeable battery, is after battery discharge, by the mode of charging, active material is activated and continue the battery of use.Relative to dry cell, the cycle charging number of times of secondary cell can reach thousands of to tens thousand of times, is a kind of novel environment-friendly battery.
Secondary cell in the market mainly comprises lead-acid battery, ickel-cadmium cell, Ni-MH battery and lithium ion battery.Lead-acid battery low price but containing the heavy metal lead of contaminated environment, ickel-cadmium cell comparatively environmental protection but energy density is lower, Ni-MH battery energy density is higher but have slight memory effect, and under hot environment, efficiency for charge-discharge is poor.Relative to lead-acid battery, ickel-cadmium cell and Ni-MH battery, lithium ion battery has higher specific energy, and discharge curve balances, and self-discharge rate is low, and cycle life is longer, memory-less effect, environmentally safe, is the green battery grown up in the last few years.
Lithium ion battery is owing to having higher energy density, long cycle life, the plurality of advantages such as lower self-discharge rate and environmental friendliness, the mobile communication equipments such as mobile phone, digital camera, notebook computer are widely used in, more be hopeful to be applied in the new-energy automobile such as hybrid vehicle (HEV) and pure electric automobile (EV), meanwhile, also placed high hopes by people in the energy storage of wind power generation or solar power generation.But if will successfully apply in these areas, lithium ion battery just must do further lifting in battery price, fail safe, useful life etc.At present, commercial lithium-ion batteries mainly adopts native graphite or modified graphite as negative material, and the theoretical specific capacity of graphite is only 372mAhg
-1, its utilance has reached its limit.Meanwhile, the intercalation potential of graphite material and the sedimentation potential of lithium metal closely, easily produce Li dendrite when high current charge-discharge, thus cause safety problem.Be difficult to the lithium ion battery growth requirement meeting high-energy-density, high security.Metallic tin has the high (994mAhg of theoretical lithium storage content
-1), the advantage such as cheap, the removal lithium embedded current potential of tin base cathode material is higher simultaneously, avoids the generation of the negative side Li dendrite when high current charge-discharge, can improve the fail safe of battery, become one of focus of high-capacity cathode material research.But tin base cathode material is in the embedding de-process of lithium, and there is larger volumetric expansion and contraction, this chaps causing material to be subject to the effect of internal stress thus cause efflorescence, inefficacy, finally causes the cycle performance of material to decline.At present, for how to suppress the volumetric expansion of kamash alloy material and shrink the key issue having become exploitation tin-based negative electrode materials for lithium-ion battery with the cycle performance improving alloy material.
Because cobalt atom has diffusion velocity and do not form carbide with carbon (if form carbide faster in tin, its metal structure can be caused to reset when Lithium-ion embeding is deviate from, thus cause structural instability, cycle performance is not good), so nowadays Sn-Co-C composite material has become the study hotspot of tin base alloy anode.
In recent years, carbothermic method is as a kind of easy, preparation that low cost, free of contamination technology have been applied to Sn-Co-C composite material.But the Sn-Co-C composite material that document is reported, still exist the comparatively complicated requirement to appointed condition of preparation process also higher and cycle characteristics also need the problems such as improvement.
Summary of the invention
In view of this, the object of the present invention is to provide the preparation method of a kind of technical process simple serondary lithium battery negative pole Sn-Co-C composite material.
For achieving the above object, the invention provides following technical scheme:
The invention provides a kind of method preparing serondary lithium battery negative pole Sn-Co-C composite material, specifically comprise the steps:
Take Xi Yuan, cobalt source and carbon source with the mol ratio of Sn:Co:C for 3:2:1, add appropriate amount of deionized water, general milling 2 ~ 5h, by described mixture calcining at constant temperature 6 ~ 12h at 700 ~ 1100 DEG C in nitrogen atmosphere, naturally, after cooling, grinding, obtains Sn-Co-C composite negative pole material.
Described carbon source is one or more the mixture in sucrose, glucose and graphite.
Preferably, described carbon source is the mixture of sucrose and graphite.
The present invention also provides a kind of serondary lithium battery, comprising: positive pole, said method prepare Sn-Co-C composite material negative pole, barrier film between a positive electrode and a negative electrode and electrolyte are set.
Preferably, described just very cobalt acid lithium, lithium nickel cobalt dioxide, nickel ion doped, the acid of nickel manganese cobalt lithium, LiMn2O4 or LiFePO4.
By the synthetic method that uses in the present invention and condition, the serondary lithium battery negative pole Sn-Co-C composite material with good cyclicity, higher specific capacity can be prepared easily and fast.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing for the present invention in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the X-ray diffractogram of the sample obtained in comparative example 1 ~ 2 of the present invention and embodiment 1 ~ 3;
Fig. 2 is the sample at room temperature cycle characteristics figure obtained in comparative example 3 ~ 4 of the present invention and embodiment 4 ~ 5.
Embodiment
The invention discloses a kind of method preparing serondary lithium battery negative pole Sn-Co-C composite material, specifically comprise the steps:
Take Xi Yuan, cobalt source and carbon source with the mol ratio of Sn:Co:C for 3:2:1, add appropriate amount of deionized water, general milling 2 ~ 5h, by described mixture calcining at constant temperature 6 ~ 12h at 700 ~ 1100 DEG C in nitrogen atmosphere, naturally, after cooling, grinding, obtains Sn-Co-C composite negative pole material.
Described carbon source is one or more the mixture in sucrose, glucose and graphite.
Preferably, described carbon source is the mixture of sucrose and graphite.
The present invention also provides a kind of serondary lithium battery, comprising: positive pole, said method prepare Sn-Co-C composite material negative pole, barrier film between a positive electrode and a negative electrode and electrolyte are set.
Preferably, described just very cobalt acid lithium, lithium nickel cobalt dioxide, nickel ion doped, the acid of nickel manganese cobalt lithium, LiMn2O4 or LiFePO4.
The present invention is not particularly limited described serondary lithium battery barrier film, considers from cost factor, is preferably polyethylene diagrams or polypropylene diaphragm.
The present invention is not particularly limited described serondary lithium battery electrolyte, the nonaqueous electrolytic solution for serondary lithium battery that can be known to the skilled person, as containing LiPF
6, LiBF
4, LiAsF
6, LiClO
4, LiCH
3sO
3, LiN (SO
2cF
3)
2, LiC (SO
2cF
3)
3, LiAlCl
4, LiSiF
6, LiB (C
6h
5)
4, one or more electrolytical nonaqueous electrolytic solutions in LiCl and LiBr, be preferably LiPF
6nonaqueous electrolytic solution.
Sn-Co-C composite material negative pole prepared by the present invention can as the negative material of column lithium ion battery, rectangular lithium ion battery and button-shaped lithium ion battery, and can as the negative material of lithium-ion-power cell and lithium-ion energy storage battery.
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be described in detail the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite not making creative work, all belongs to the scope of protection of the invention.
Comparative example 1
Weigh Xi Yuan, cobalt source and graphite with the mol ratio of Sn:Co:C for 3:2:1, add appropriate amount of deionized water, with general milling 5h, by described mixture in nitrogen atmosphere with 700 DEG C of calcining at constant temperature 12h, naturally, after cooling, grinding, obtaining take graphite as the Sn-Co-C composite material of carbon source.
Comparative example 2
Weigh Xi Yuan, cobalt source and sucrose with the mol ratio of Sn:Co:C for 3:2:1, add appropriate amount of deionized water, with general milling 2h, by described mixture in nitrogen atmosphere with 1100 DEG C of calcining at constant temperature 6h, naturally, after cooling, grinding, obtaining take sucrose as the Sn-Co-C composite material of carbon source.
Embodiment 1
With the mol ratio of Sn:Co:C for 3:2:1 weighs Xi Yuan, cobalt source, sucrose and graphite (carbon atomic ratio of sucrose and graphite is for 1:1), add appropriate amount of deionized water, with general milling 4h, by described mixture in nitrogen atmosphere with 900 DEG C of calcining at constant temperature 10h, naturally after cooling, grinding, the Sn-Co-C composite material that to obtain with sucrose and graphite be compounded carbons.
Embodiment 2
With the mol ratio of Sn:Co:C for 3:2:1 weighs Xi Yuan, cobalt source, sucrose and graphite (carbon atomic ratio of sucrose and graphite is for 2:1), add appropriate amount of deionized water, with general milling 3h, by described mixture in nitrogen atmosphere with 800 DEG C of calcining at constant temperature 11h, naturally after cooling, grinding, the Sn-Co-C composite material that to obtain with sucrose and graphite be compounded carbons.
Embodiment 3
With the mol ratio of Sn:Co:C for 3:2:1 weighs Xi Yuan, cobalt source, sucrose and graphite (carbon atomic ratio of sucrose and graphite is for 1:2), add appropriate amount of deionized water, with general milling 3.5h, by described mixture in nitrogen atmosphere with 1000 DEG C of calcining at constant temperature 8h, naturally after cooling, grinding, the Sn-Co-C composite material that to obtain with sucrose and graphite be compounded carbons.
As can be seen from Figure 1, no matter be comparative example 1 ~ 2, or embodiment 1 ~ 3, according to the sample that the experiment route of our design obtains, all containing CoSn, CoSn2, CoSn3, Sn phase in their X ray diffracting spectrum, except comparative example 2, other all have the diffraction maximum of graphite.
Embodiment 4
Sample embodiment 1 prepared mixes in 8:1:1 ratio with conductive black super P, binding agent PVDF, be dissolved in 1-METHYLPYRROLIDONE (NMP), be coated in after stirring on Copper Foil and make negative plate, by described negative plate in vacuum drying oven at 120 DEG C dry 12h, dried negative plate, positive pole, polypropylene diaphragm and the electrolyte prepared with LiFePO4 are assembled in the glove box being full of high-purity argon gas, obtains CR2032 type button experimental cell.
Discharging current is 100 milliamperes every gram, and charging current is 100 milliamperes every gram, and charging/discharging voltage is interval between 0.01 ~ 3.0 volt.In described electrolyte, supporting electrolyte is LiPF
6, to be ethylene carbonate (EC) with diethyl carbonate (DEC) be solvent by volume mixes at 1: 1, and the concentration of described electrolyte is 1mol/L, and battery testing temperature is room temperature.
Embodiment 5
Sample embodiment 2 prepared mixes in 8:1:1 ratio with conductive black super P, binding agent PVDF, be dissolved in 1-METHYLPYRROLIDONE (NMP), be coated in after stirring on Copper Foil and make negative plate, by described negative plate in vacuum drying oven at 120 DEG C dry 12h, dried negative plate, positive pole, polypropylene diaphragm and the electrolyte prepared with LiFePO4 are assembled in the glove box being full of high-purity argon gas, obtains CR2032 type button experimental cell.
Discharging current is 100 milliamperes every gram, and charging current is 100 milliamperes every gram, and charging/discharging voltage is interval between 0.01 ~ 3.0 volt.In described electrolyte, supporting electrolyte is LiPF
6, to be ethylene carbonate (EC) with diethyl carbonate (DEC) be solvent by volume mixes at 1: 1, and the concentration of described electrolyte is 1mol/L, and battery testing temperature is room temperature.
Comparative example 3
The sample prepared by comparative example 1 mixes in 8:1:1 ratio with conductive black super P, binding agent PVDF, be dissolved in 1-METHYLPYRROLIDONE (NMP), be coated in after stirring on Copper Foil and make negative plate, by described negative plate in vacuum drying oven at 120 DEG C dry 12h, dried negative plate, positive pole, polypropylene diaphragm and the electrolyte prepared with LiFePO4 are assembled in the glove box being full of high-purity argon gas, obtains CR2032 type button experimental cell.
Discharging current is 100 milliamperes every gram, and charging current is 100 milliamperes every gram, and charging/discharging voltage is interval between 0.01 ~ 3.0 volt.In described electrolyte, supporting electrolyte is LiPF
6, to be ethylene carbonate (EC) with diethyl carbonate (DEC) be solvent by volume mixes at 1: 1, and the concentration of described electrolyte is 1mol/L, and battery testing temperature is room temperature.
Comparative example 4
The sample prepared by comparative example 2 mixes in 8:1:1 ratio with conductive black super P, binding agent PVDF, be dissolved in 1-METHYLPYRROLIDONE (NMP), be coated in after stirring on Copper Foil and make negative plate, by described negative plate in vacuum drying oven at 120 DEG C dry 12h, dried negative plate, positive pole, polypropylene diaphragm and the electrolyte prepared with LiFePO4 are assembled in the glove box being full of high-purity argon gas, obtains CR2032 type button experimental cell.
Discharging current is 100 milliamperes every gram, and charging current is 100 milliamperes every gram, and charging/discharging voltage is interval between 0.01 ~ 3.0 volt.In described electrolyte, supporting electrolyte is LiPF
6, to be ethylene carbonate (EC) with diethyl carbonate (DEC) be solvent by volume mixes at 1: 1, and the concentration of described electrolyte is 1mol/L, and battery testing temperature is room temperature.
As can be seen from Figure 2, by the sample that comparative example 3 and comparative example 4 obtain, under the current density of 100 milliamperes every gram, first discharge specific capacity is 523 Milliampere Hours every gram and 639 Milliampere Hours every gram, after 40 circles, its specific discharge capacity is only 215 Milliampere Hours every gram and 354 Milliampere Hours every gram, its capacity attenuation or obvious.And pass through the sample of embodiment 4 and embodiment 5 acquisition, under the current density of 100 milliamperes every gram, first discharge specific capacity is respectively 634 Milliampere Hours every gram and 618 Milliampere Hours every gram, after 40 circles, its specific discharge capacity still has 488 Milliampere Hours and 609 Milliampere Hours every gram, its special capacity fade is slow, and specific capacity all higher than the sample that comparison specimen is obtained, has showed good cycle performance.
Can say, utilize the Sn-Co-C composite negative pole material that sucrose and graphite are prepared for compounded carbons, not only increase its specific discharge capacity, effectively can also improve the deficiencies such as tin base cathode material cycle performance difference, therefore this system material is a kind of novel high-performance negative material.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.Any Reference numeral in claim should be considered as the claim involved by limiting.
In addition, be to be understood that, although this specification is described according to execution mode, but not each execution mode only comprises an independently technical scheme, this narrating mode of specification is only for clarity sake, those skilled in the art should by specification integrally, and the technical scheme in each embodiment also through appropriately combined, can form other execution modes that it will be appreciated by those skilled in the art that.
Claims (3)
1. a preparation method for serondary lithium battery negative pole Sn-Co-C composite material, is characterized in that, comprise the steps:
Take Xi Yuan, cobalt source and carbon source with the mol ratio of Sn:Co:C for 3:2:1, add appropriate amount of deionized water, general milling 2 ~ 5h, by described mixture calcining at constant temperature 6 ~ 12h at 700 ~ 1100 DEG C in nitrogen atmosphere, naturally, after cooling, grinding, obtains Sn-Co-C composite negative pole material; Wherein, described carbon source is the mixture of sucrose and graphite.
2. a serondary lithium battery, is characterized in that, comprising: positive pole, method according to claim 1 prepare Sn-Co-C composite material negative pole, barrier film between a positive electrode and a negative electrode and electrolyte are set.
3. serondary lithium battery according to claim 2, is characterized in that: described just very cobalt acid lithium, lithium nickel cobalt dioxide, nickel ion doped, the acid of nickel manganese cobalt lithium, LiMn2O4 or LiFePO4.
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