CN105810936A - Layered structured negative electrode material Ca9Co12O28 of lithium ion battery and preparation method of layered structure negative electrode material - Google Patents
Layered structured negative electrode material Ca9Co12O28 of lithium ion battery and preparation method of layered structure negative electrode material Download PDFInfo
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- CN105810936A CN105810936A CN201610013546.XA CN201610013546A CN105810936A CN 105810936 A CN105810936 A CN 105810936A CN 201610013546 A CN201610013546 A CN 201610013546A CN 105810936 A CN105810936 A CN 105810936A
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- lithium ion
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- ion battery
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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
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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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- 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 layered structured negative electrode material Ca9Co12O28 of a lithium ion battery and a preparation method of the layered structure negative electrode material, relating to the field of the lithium ion battery. The method comprises the following steps of mixing and dissolving 1 part of calcium source, 1-2 parts of cobalt sources and 0.005-0.01 part of surfactant in water according to the mole part, and enabling the mixture to react for 1.5-3 hours at 35-45 DEG C; adding 4-5 parts of weak acid, rising a temperature to 47-55 DEG C for reaction for 1.5-3 hours, adding 18-20 parts of polyalcohol, rising the temperature to 70-85 DEG C for reaction for 1.5-3 hours, and carrying out reduced pressure distillation to remove moisture; and carrying out reaction for 3-5 hours at 140-160 DEG C, and calcining resin for 3-5 hours at 800-900 DEG C. The Ca9Co12O28 is of a layered structure, the grain size is 0.5-1.2 micrometers, and the discharging specific capacity is maintained at 236mAh g<-1> after the Ca9Co12O28 is charged and discharged for 200 times in a condition that the current density is 1,800-2,000mAh g<-1>. The Ca9Co12O28 disclosed by the invention is uniform in size, the rate performance of the electrode material can be improved, and rapid charging and discharging is achieved.
Description
Technical field
The present invention relates to field of lithium, be specifically related to the lithium ion battery negative material Ca of a kind of layer structure9Co12O28And preparation method thereof.
Background technology
Owing to conventional fossil fuel is non-renewable energy resources, storage capacity is limited, and pollutes the environment during using, it is impossible to meet the human development needs to the energy, therefore, is permitted to develop new cleaning, green, environmental protection, the reproducible energy energy as an alternative.
Lithium ion battery (hereinafter referred to as lithium battery) with its light weight, specific energy is high, have extended cycle life the features such as environmental protection, rapidly becomes the emphasis of the main research and development of the rechargeable formula power supply of portable type electronic product.
Existing lithium battery generally uses material with carbon element to be negative material, and the theoretical capacity of material with carbon element is 372mAh g-1But, the power density of material with carbon element is relatively low, it is difficult to meeting the demand of large-capacity high-power power supply such as electric automobile, at present, Si, transition metal oxide and derivant thereof become the potential replacement person of lithium cell cathode material.
Ca9Co12O28A kind of stratiform cobalt oxide, it at high temperature stable chemical nature, toxicity low, cheap, its theoretical capacity is up to 636mAh g-1.Research shows, Ca9Co12O28In charge and discharge process, can generate inactive solid CaO, solid CaO can support active substance as framing structure, reduces the change in volume of negative material, and then the integrity of holding electrode material, embodies preferable chemical property.
Ca9Co12O28Crystal structure and Ca2Co2O5Material is closely similar, by CoO2Layer and rock salt CaO layer are alternately stacked and form layer structure, but Ca9Co12O28In comprise orderly oxygen vacancy.
Ca9Co12O28Generally use high temperature solid-solid reaction method, coprecipitation or the synthesis of Pechini (Via Polymeric Precursor Method) method, high temperature solid-solid reaction method and coprecipitation can not control product morphology and grain size, and high-temperature calcination can cause product grain to be reunited for a long time, forms irregular micron order product；Although Pechini method can obtain even-grained nano-particle, effectively shortening lithium ion the evolving path, but the Ca obtained9Co12O28Granule is too small, increases Ca9Co12O28With the contact area of electrolyte, cause the formation of large-area solid electrolyte interface film, consume part lithium ion so that first charge-discharge irreversible capacity increases, and reduces the efficiency for charge-discharge of electrode material；And owing to big contact area causes active substance to be easily soluble in electrolyte, make battery capacity rapid decay in charge and discharge process.
Summary of the invention
For defect present in prior art, it is an object of the invention to provide the lithium ion battery negative material Ca of a kind of layer structure9Co12O28And preparation method thereof, it is possible to obtain size uniform, and the suitable Ca of particle diameter9Co12O28。Ca9Co12O28, when using as negative material, it is possible to increase the high rate performance of electrode material, it is achieved fast charging and discharging.
For reaching object above, the present invention adopts the technical scheme that:
A kind of lithium ion battery negative material Ca of layer structure9Co12O28Preparation method, comprise the following steps；
A, by molar part, 1 part of calcium source, 1～2 part of cobalt source mixed with 0.005～0.01 part of surfactant and be dissolved in water, under conditions of reaction temperature is 35～45 DEG C, reacting 1.5～3h；
B, 4～5 parts of weak acid of addition, be warming up to 47～55 DEG C of reactions 1.5～3h, be subsequently adding 18～20 parts of polyhydric alcohol, is warming up to 70～85 DEG C of reactions 1.5～3h, and decompression is distilled off moisture；
C, reaction 3～5h at 140～160 DEG C, obtain solid polymer resin, resin finally calcined at 800～900 DEG C 3～5h.
On the basis of technique scheme, the reaction temperature in described step a is 40 DEG C.
On the basis of technique scheme, described step b comprises the following steps: add 4～5 parts of weak acid, is warming up to 50 DEG C of reaction 2h.
On the basis of technique scheme, described step b comprises the following steps: add 18～20 parts of polyhydric alcohol, is warming up to 80 DEG C of reaction 2h.
On the basis of technique scheme, described calcium source is that calcium chloride, calcium nitrate, the hydrate of calcium chloride or the hydrate of calcium nitrate are selected in described calcium source.
On the basis of technique scheme, described cobalt source is CoF2, CoCl2, CoBr2, CoI2, Co (NO3)2, CoSO4In any one, or the above-mentioned corresponding hydrated salt of any one salt.
On the basis of technique scheme, described weak acid is citric acid.
On the basis of technique scheme, described polyhydric alcohol is ethylene glycol, 2 one propylene glycol, BDO or glycerol.
On the basis of technique scheme, described surfactant is sodium lauryl sulphate, dodecylbenzene sodium sulfonate, cetyl trimethylammonium bromide or hexadecyltrimethylammonium chloride.
On the basis of technique scheme, described weak acid: metal ion: the mol ratio of polyhydric alcohol is 2:1:8, described metal ion is the calcium ion in calcium source and the cobalt ion sum in cobalt source.
A kind of Ca using method according to any one of claim 1 to 8 to prepare9Co12O28, described Ca9Co12O28For layer structure, particle diameter is for for 0.5～1.2 μm, being 1800～2000mAh g in electric current density-1Under conditions of, after discharge and recharge 200 times, specific discharge capacity still has 236mAh g-1。
Compared with prior art, it is an advantage of the current invention that:
(1) the lithium ion battery negative material Ca of a kind of layer structure of the present invention9Co12O28And preparation method thereof include the addition of surfactant, metal-weak acid chelate is made to be frozen in polymer network the original metal ion proportioning kept in initial soln, reach the mixing of atomic level, it is ensured that the chemical reaction uniformity of intermediate product presoma.
And shorten calcination time, provide guarantee for stable product pattern further；On the other hand, surfactant not only makes the dispersibility of each microgranule in solution more preferable, granule is evenly, lithium ion is facilitated to spread, kinetically, lithium is propagated faster, can realize fast charging and discharging, and surfactant can simultaneously serve as end-capping reagent, stablize the microgranule in solution, controlling particle size, compare the nanosized product that Pechini method obtains, this method products therefrom particle size is moderate, it is unlikely to the least, the least side reaction probability that can improve, is also unlikely to too big, and too conference reduces lithium ion the evolving path.
Accompanying drawing explanation
Fig. 1 is negative material Ca in the embodiment of the present invention9Co12O28Electron-microscope scanning figure；
Fig. 2 is negative material Ca9Co12O28EDS figure；
Fig. 3 is negative material Ca9Co12O28Charge and discharge electrograph under 3C multiplying power；
Fig. 4 is negative material Ca9Co12O28The cycle performance figure of 200 times is circulated under 3C multiplying power；
Fig. 5 is negative material Ca9Co12O28Performance map under different multiplying.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Shown in Figure 1, the embodiment of the present invention provides the lithium ion battery negative material Ca of a kind of layer structure9Co12O28Preparation method, comprise the following steps:
S1, by molar part, by 1 part of calcium source, 1～2 part of cobalt source and 0.005～0.01 part of surfactant are blended and dissolved in suitable quantity of water that (water is used as solvent, its addition is determined according to actual needs, do not specially require), 1.5～3h (optimum for 2h) are reacted under conditions of temperature is 35～45 DEG C (optimum is 40 DEG C), add 4～5 parts of weak acid, after being warming up to 47～55 DEG C (optimum is 50 DEG C) reaction 1.5～3h (optimum for 2h), add 18～20 parts of polyhydric alcohol, it is warming up to 70～85 DEG C (optimum is 80 DEG C), reaction 1.5～3h (optimum is 2h), obtain crude product.
S2, regulating vacuum distillation temperature according to vacuum, decompression is distilled off moisture, at 140～160 DEG C (optimum is 150 DEG C), in fume hood heat treatment 3～5h (optimum for 4h) to NO2Release completely, polyhydric alcohol is made to be polymerized further with chelate, obtain solid polymer resin, finally by fluoropolymer resin high-temperature calcination 3～5h (optimum for 4h) under 800～900 DEG C (optimum is 850 DEG C), after cooling, obtain calcium cobalt oxide negative material.
In actual production, citric acid, metal ion total amount, the mol ratio of ethylene glycol can be adjusted according to actual needs, in the present embodiment, citric acid, metal ion total amount, the mol ratio of ethylene glycol are 2:1:8, wherein, the calcium ion during metal ion total amount is calcium source and the cobalt ion sum in cobalt source.
In the embodiment of the present invention, soluble calcium salt is selected in calcium source, can be calcium chloride, calcium nitrate, the hydrate of calcium chloride or the hydrate of calcium nitrate, and in the present embodiment, calcium source is Ca (NO3)2·4H2O。
In the embodiment of the present invention, cobalt source selects soluble cobalt, can be CoF2, CoCl2, CoBr2, CoI2, Co (NO3)2, CoSO4In any one, or the above-mentioned corresponding hydrated salt of any one salt, in the present embodiment, cobalt source is Co (NO3)2·6H2O。
Surfactant can be sodium lauryl sulphate, dodecylbenzene sodium sulfonate, cetyl trimethylammonium bromide or hexadecyltrimethylammonium chloride.In the present embodiment, sodium lauryl sulphate selected by surfactant.
Weak acid selects citric acid.
Polyhydric alcohol selects ethylene glycol, 2 one propylene glycol, BDO or glycerol, and the polyhydric alcohol in the present embodiment is ethylene glycol.
In the present invention, surfactant is added on the basis of Pechini method, make metal-weak acid chelate be frozen in polymer network the original metal ion proportioning kept in initial soln, reach the mixing of atomic level, it is ensured that the chemical reaction uniformity of intermediate product presoma.
And shorten calcination time, provide guarantee for stable product pattern further；On the other hand, surfactant not only makes the dispersibility of each microgranule in solution more preferable, granule is evenly, lithium ion is facilitated to spread, kinetically, lithium is propagated faster, can realize fast charging and discharging, and surfactant can simultaneously serve as end-capping reagent, stablize the microgranule in solution, controlling particle size, compare the nanosized product that Pechini method obtains, this method products therefrom particle size is moderate, it is unlikely to the least, the least side reaction probability that can improve, is also unlikely to too big, and too conference reduces lithium ion the evolving path.
Use the Ca that said method is made9Co12O28, its chemical property is: under the conditions of multiplying power is 3C (or be 1800～2000mAh g in electric current density-1Under conditions of) specific discharge capacity is maintained at 236mAh g after discharge and recharge 200 times-1, have preferable cyclical stability.
Ca shown in Figure 1, in the present invention9Co12O28Having layer structure clearly, size ratio is more uniform, is 0.5～1.2 μm.
Shown in Figure 2, for the EDS (Energy Dispersive Spectroscopy, dispersion spectrogram) of product, it can be seen that the composition in product and molecular formula Ca9Co12O28Match, illustrate that the product using said method synthesis is Ca9Co12O28。
See Fig. 3, shown in 4, for Ca9Co12O28Charge and discharge electrograph under 3C multiplying power, cycle performance figure, from the figure 3, it may be seen that the Ca of the present invention9Co12O28When being used as lithium cell cathode material, under the electric current density of 3C, good rate capability.See Fig. 4 to understand, the Ca of the present invention9Co12O28When being used as lithium cell cathode material, after carrying out repeatedly discharge and recharge under higher electric current density, still there is preferable efficiency for charge-discharge；Shown in Figure 5, the Ca of the present invention9Co12O28When being used as lithium cell cathode material, being respectively provided with preferable performance under the electric current density of different multiplying, range of application is wider.
The present invention is not limited to above-mentioned embodiment, for those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications, within these improvements and modifications are also considered as protection scope of the present invention.The content not being described in detail in this specification belongs to prior art known to professional and technical personnel in the field.
Claims (10)
1. the lithium ion battery negative material Ca of a layer structure9Co12O28Preparation method,
It is characterized in that: comprise the following steps；
A, by molar part, by 1 part of calcium source, 1～2 part of cobalt source and 0.005～0.01 part of surface
Activating agent mixes and is dissolved in water, reacts under conditions of reaction temperature is 35～45 DEG C
1.5～3h；
B, 4～5 parts of weak acid of addition, be warming up to 47～55 DEG C of reactions 1.5～3h, be subsequently adding
18～20 parts of polyhydric alcohol, are warming up to 70～85 DEG C of reactions 1.5～3h, and decompression is distilled off moisture；
C, reaction 3～5h at 140～160 DEG C, obtain solid polymer resin, finally will
Resin calcines 3～5h at 800～900 DEG C.
The lithium ion battery negative material of a kind of layer structure the most as claimed in claim 1
Ca9Co12O28And preparation method thereof, it is characterised in that: the reaction temperature in described step a is
40℃。
The lithium ion battery negative material of a kind of layer structure the most as claimed in claim 1
Ca9Co12O28And preparation method thereof, it is characterised in that: described step b comprises the following steps:
Add 4～5 parts of weak acid, be warming up to 50 DEG C of reaction 2h, add 18～20 parts of polyhydric alcohol, rise
Temperature reacts 2h to 80 DEG C.
The lithium ion battery negative material of a kind of layer structure the most as claimed in claim 1
Ca9Co12O28And preparation method thereof, it is characterised in that: described calcium source is that chlorine is selected in described calcium source
Change calcium, calcium nitrate, the hydrate of calcium chloride or the hydrate of calcium nitrate.
The lithium ion battery negative material of a kind of layer structure the most as claimed in claim 1
Ca9Co12O28And preparation method thereof, it is characterised in that: described cobalt source is CoF2, CoCl2,
CoBr2, CoI2, Co (NO3)2, CoSO4In any one, or any one salt phase above-mentioned
The hydrated salt answered.
The lithium ion battery negative material of a kind of layer structure the most as claimed in claim 1
Ca9Co12O28And preparation method thereof, it is characterised in that: described weak acid is citric acid.
The lithium ion battery negative material of a kind of layer structure the most as claimed in claim 1
Ca9Co12O28And preparation method thereof, it is characterised in that: described polyhydric alcohol be ethylene glycol, 2 one
Propylene glycol, BDO or glycerol.
The lithium ion battery negative material of a kind of layer structure the most as claimed in claim 1
Ca9Co12O28And preparation method thereof, it is characterised in that: described surfactant is dodecyl
Sodium sulfate, dodecylbenzene sodium sulfonate, cetyl trimethylammonium bromide or cetyl front three
Ammonium chloride.
9. the lithium-ion electric of a kind of layer structure as according to any one of claim 1 to 7
Pond negative material Ca9Co12O28And preparation method thereof, it is characterised in that: described weak acid: metal
Ion: the mol ratio of polyhydric alcohol is 2:1:8, described metal ion be calcium ion in calcium source with
Cobalt ion sum in cobalt source.
10. one kind uses method according to any one of claim 1 to 8 to prepare
Ca9Co12O28, it is characterised in that: described Ca9Co12O28For layer structure, particle diameter be 0.5～
1.2 μm, are 1800～2000mAg in electric current density-1Under conditions of, after discharge and recharge 200 times
Specific discharge capacity is maintained at 236mAhg-1。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100994269B1 (en) * | 2007-07-11 | 2010-11-12 | 한국과학기술연구원 | New calcium-cobalt oxide anode materials and method for manufacturing the same |
| CN103746092A (en) * | 2013-12-20 | 2014-04-23 | 中国东方电气集团有限公司 | Preparation method of calcium-cobalt oxide compound as anode material for lithium ion batteries |
| CN104659359A (en) * | 2015-02-15 | 2015-05-27 | 湘潭大学 | Preparation method of nanometer plate overlaid and stacked cube Mn<3-x>CoxO4 negative material of lithium-ion battery |
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2016
- 2016-01-11 CN CN201610013546.XA patent/CN105810936B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100994269B1 (en) * | 2007-07-11 | 2010-11-12 | 한국과학기술연구원 | New calcium-cobalt oxide anode materials and method for manufacturing the same |
| CN103746092A (en) * | 2013-12-20 | 2014-04-23 | 中国东方电气集团有限公司 | Preparation method of calcium-cobalt oxide compound as anode material for lithium ion batteries |
| CN104659359A (en) * | 2015-02-15 | 2015-05-27 | 湘潭大学 | Preparation method of nanometer plate overlaid and stacked cube Mn<3-x>CoxO4 negative material of lithium-ion battery |
Non-Patent Citations (1)
| Title |
|---|
| TAO MEI等: ""Preparation of mixed oxides Ca9Co12O28 and their electrochemical properties"", 《MATERIALS LETTERS》 * |
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