CN102583583B - A kind of lithium ion battery manganese cobalt lithium oxide anode material and preparation method thereof - Google Patents
A kind of lithium ion battery manganese cobalt lithium oxide anode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of lithium ion battery manganese cobalt lithium oxide anode material and preparation method thereof.The chemical formula of this positive electrode is represented by: Li(3+x)/3Mn2x/3Co1-xO2, wherein 0.1≤x≤0.9.This positive electrode has a height ratio capacity and high/low temperature such as is suitable at the excellent chemical property.This preparation method is characterised by simple to operate, production cost is low, synthesis cycle is short and repeatability is high；Do not introduce foreign ion, make product purity be greatly improved；Lithium ion and transition metal ions coprecipitation, various Ar ion mixings are more uniform；The method can be widely applied to the synthesis of lithium ion battery oxide anode material.
Description
Technical field
The present invention relates to a kind of manganese cobalt oxidate for lithium positive electrode in field of lithium ion battery and preparation method thereof, the chemical formula of this positive electrode is represented by: Li(3+x)/3Mn2x/3Co1-xO2, wherein 0.1≤x≤0.9.
Background technology
Due to lithium ion battery there is high voltage, high power capacity, have extended cycle life, the advantage such as good, the environmental protection of security performance, be widely used to the fields such as portable electric appts, power set, Aero-Space, space technology.Coprecipitation, in the synthesis of lithium ion battery transition metal oxide positive electrode, has great advantage: (1) product particle is uniformly dispersed, and particle size distribution is homogeneous；(2) technical process is simple, it is easy to control, it is easy to large-scale production；(3) simple to producing equipment requirements, production cost is low.Although traditional coprecipitation (with NaOH for precipitant) has many advantages, but there is very big weak point.Such as: (1) first prepares transition metal hydroxide predecessor then the technique mixed with lithium salts, not only makes production complicate, and is unfavorable for the uniformity of product；(2) in order to form the coprecipitated thing of transition metal, it has to add precipitant when gas shield, so make again to produce to complicate, improve production cost, and be unfavorable for large-scale production；(3) supersaturation different between transition metal hydroxide causes that presoma phase composition is fluctuated, and makes coprecipitation process poor repeatability；(4) foreign ion Na is inevitably introduced with NaOH for precipitant+, improve the water absorption of product, make the chemical property of positive electrode worsen.But, the method that the present invention adopts, the perfect above-mentioned deficiency solved, further simplify production technology, improve the performance of product.Adopting material prepared by the inventive method, excellent product performance, technical process is simple, it is easy to controlling, reproducible, cost is low, has heavy industrialization application prospect.
Summary of the invention
It is an object of the invention to provide a kind of lithium ion battery manganese cobalt lithium oxide anode material and preparation method thereof, the chemical formula of this positive electrode is represented by: Li(3+x)/3Mn2x/3Co1-xO2, wherein 0.1≤x≤0.9.
Li provided by the present invention(3+x)/3Mn2x/3Co1-xO2Positive electrode, as the positive electrode of lithium ion battery, not only has excellent chemical property, and also has excellent chemical property under high/low temperature condition during room temperature.
Li provided by the invention(3+x)/3Mn2x/3Co1-xO2The preparation method of positive electrode comprises the following steps:
(1) first weighing lithium salts, manganese salt and cobalt salt, the ratio making metal ion Li: Mn: Co is 1.033: 0.067: 0.9～1.3: 0.6: 0.1, the slaine weighed is dissolved in dehydrated alcohol, obtains alcoholic solution；
(2) weigh the oxalic acid measuring ratio little over quantification chemistry, and be dissolved in dehydrated alcohol, and add in the alcoholic solution that step (1) obtains, sucking filtration drying after stirring, obtain (LiMnCo)xC2O4Presoma；
(3) (LiMnCo) that step (2) is obtainedxC2O4After presoma carries out heat treatment and cooling process, it is thus achieved that Li(3+x)/3Mn2x/3Co1-xO2Positive electrode powder.
Lithium salts in above-mentioned steps (1) is one or more in Quilonorm (SKB), lithium nitrate, lithium chloride；Manganese salt is one or more in manganese acetate, manganese nitrate, manganese chloride；Cobalt salt is one or more in cobalt acetate, cobalt nitrate, cobaltous chloride；
The presoma of step (2) gained is the coprecipitated thing of lithium ion and transition metal ions, and mixing time is 0.5h～2h；
In step (3), heat treatment temperature is 800 DEG C～1000 DEG C, time 3～16h；Cooling processing mode is quenching in quenching, mixture of ice and water in quenching, liquid nitrogen under room temperature.
The present invention adopts coprecipitation to prepare Li(3+x)/3Mn2x/3Co1-xO2Positive electrode, with dehydrated alcohol for solvent, oxalic acid is precipitant, makes lithium ion and transition metal ions form coprecipitated thing, solve lithium ion in conventional coprecipitation to fail to form the problem of coprecipitated thing with transition metal ions, substantially increase the degree that is uniformly dispersed and the homogeneity of product；The method that the present invention adopts does not introduce foreign ion, greatly enhances the purity of product, solves the problem that material property is worked the mischief by foreign ion；Additionally, the method that the present invention takes, shorten processing step greatly, saved ample resources, contribute to sequencing and produce, saved production cost.The raw material sources that the present invention adopts are extensive, and process engineering is simple, it is easy to control, reproducible, it is possible to scale synthesizes.The synthetic method that the present invention adopts is not limited to the material that the present invention announces, it is also possible to for the synthesis of other materials, the method has broad application prospects.
Accompanying drawing explanation
Fig. 1 is embodiment 1Li1.2Mn0.4Co0.4O2The X-ray diffracting spectrum of positive electrode powder body.
Fig. 2 is embodiment 1Li1.2Mn0.4Co0.4O2The SEM figure of positive electrode powder body.
Fig. 3 is that embodiment 1 uses Li1.2Mn0.4Co0.4O2Positive electrode powder body is as positive pole at room temperature 20mAg-1, 60mAg-1, 100mAg-1, 200mAg-1Time charging and discharging curve.
Fig. 4 is that embodiment 1 uses Li1.2Mn0.4Co0.4O2Positive electrode powder body is as positive pole at room temperature 20mAg-1, 60mAg-1, 100mAg-1, 200mAg-1Time cycle performance curve.
Detailed description of the invention
The main implementation process of the present invention is:
(1) first weighing a certain amount of lithium salts, manganese salt and cobalt salt, the ratio making metal ion Li:Mn:Co is 1.033: 0.067: 0.9～1.3: 0.6: 0.1, the slaine weighed is dissolved in dehydrated alcohol, obtains alcoholic solution；
(2) weigh the oxalic acid measuring ratio little over quantification chemistry, and be dissolved in dehydrated alcohol, and add in the alcoholic solution obtained in step (1), sucking filtration drying after stirring certain time, obtain (LiMnCo)xC2O4Presoma；
(3) (LiMnCo) that step (2) is obtainedxC2O4After presoma carries out heat treatment and carries out cooling process, it is thus achieved that Li(3+x)/3Mn2x/3Co1-xO2Positive electrode powder.
It is further elucidated with the feature of the present invention below by way of example, but is not limited to embodiment.
Experimental technique in following embodiment, if no special instructions, is conventional method.
Embodiment 1:Li1.2Mn0.4Co0.4O2Positive electrode
With Quilonorm (SKB), manganese acetate, cobalt acetate and oxalic acid for initiation material, 0.9804g manganese acetate, 0.9964g cobalt acetate, 1.2855g Quilonorm (SKB) are dissolved in dehydrated alcohol, obtain the metal salt solution of ethanol；Again the oxalic acid 2.1634g of than stoichiometric proportion excessive 20% is dissolved in dehydrated alcohol；The alcoholic solution of oxalic acid is added in the metal salt solution of ethanol, sucking filtration be ground into powder after 100 DEG C of dry 3h and load crucible after stirring 1h；It is warmed up at 900 DEG C with the programming rate of 4 DEG C/min in batch-type furnace and heats 12h, and in annealing at room temperature, Li can be obtained1.2Mn0.4Co0.4O2Powder body material.The XRD test result of powder body material shows, the powder body of synthesis has layered rock salt structure (R3m), as shown in Figure 1.The SEM test result of powder body material shows, the powder granule of synthesis is evenly distributed, and size is 300～500nm, as shown in Figure 2.Adopting button cell to test, the mass ratio of mixed powder, conductive carbon black and binding agent PVDF (Kynoar) is 8: 1: 1, and metal lithium sheet is to pole, 1mol L-1LiPF6/ EC+DMC+EMC (volume ratio 1: 1: 1) is electrolyte, and polypropylene material is barrier film, and battery test system is NEWARETC53, and charging/discharging voltage window is 2.0～4.6V, and charging and discharging currents density chooses 20mA g respectively-1、60mA·g-1、100mA·g-1、200mA·g-1, when this material is as the positive pole of lithium ion battery, show good chemical property.Button cell test result shows, (1) is at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and 28 DEG C at first discharge specific capacity respectively 270mAh g-1、250mAh·g-1、238mAh·g-1、202mAh·g-1, as shown in Figure 3；After 28 discharge and recharges, their specific discharge capacity respectively 224mAh g-1、198mAh·g-1、173mAh·g-1、164mAh·g-1, as shown in Figure 4.(2) at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and-10 DEG C at first discharge specific capacity respectively 189mAh g-1、162mAh·g-1、141mAh·g-1、123mAh·g-1, after 28 discharge and recharges, their specific discharge capacity respectively 175mAh g-1、152mAh·g-1、129mAh·g-1、117mAh·g-1.(3) at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and 45.4 DEG C at first discharge specific capacity respectively 293mAh g-1、250mAh·g-1、248mAh·g-1、211mAh·g-1；After 28 discharge and recharges, their specific discharge capacity respectively 235mAh g-1、198mAh·g-1、199mAh·g-1、159mAh·g-1。
Embodiment 2:Li1.033Mn0.067Co0.9O2Positive electrode
With Quilonorm (SKB), manganese acetate, cobalt acetate and oxalic acid for initiation material, 0.3270g manganese acetate, 4.4836g cobalt acetate, 2.5305g Quilonorm (SKB) are dissolved in dehydrated alcohol, obtain the metal salt solution of ethanol；Again the oxalic acid 4.8021g of than stoichiometric proportion excessive 20% is dissolved in dehydrated alcohol；The alcoholic solution of oxalic acid is added in the metal salt solution of ethanol, sucking filtration be ground into powder after 100 DEG C of dry 3h and load crucible after stirring 1h；It is warmed up at 900 DEG C with the programming rate of 4 DEG C/min in batch-type furnace and heats 12h, and in annealing at room temperature, Li can be obtained1.033Mn0.067Co0.9O2Powder body material.The XRD test result of powder body material shows, the powder body of synthesis has layered rock salt structure (R3m).The SEM test result of powder body material shows, the powder granule of synthesis is evenly distributed, and size is 300～500nm.Adopting button cell to test, the mass ratio of mixed powder, conductive carbon black and binding agent PVDF (Kynoar) is 8: 1: 1, and metal lithium sheet is to pole, 1mol L-1LiPF6/ EC+DMC+EMC (volume ratio 1: 1: 1) is electrolyte, and polypropylene material is barrier film, and battery test system is NEWARETC53, and charging/discharging voltage window is 2.0～4.6V, and charging and discharging currents density chooses 20mA g respectively-1、60mA·g-1、100mA·g-1、200mA·g-1, when this material is as the positive pole of lithium ion battery, show good chemical property.Button cell test result shows, (1) is at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and 28 DEG C at first discharge specific capacity respectively 205mAh g-1、185mAh·g-1、166mAh·g-1、143mAh·g-1；After 28 discharge and recharges, their specific discharge capacity respectively 186mAh g-1、162mAh·g-1、149mAh·g-1、131mAh·g-1.(2) at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and-10 DEG C at first discharge specific capacity respectively 173mAh g-1、155mAh·g-1、136mAh·g-1、121mAh·g-1, after 28 discharge and recharges, their specific discharge capacity respectively 165mAh g-1、146mAh·g-1、127mAh·g-1、114mAh·g-1.(3) at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and 45.4 DEG C at first discharge specific capacity respectively 236mAh g-1、212mAh·g-1、196mAh·g-1、178mAh·g-1；After 28 discharge and recharges, their specific discharge capacity respectively 204mAh g-1、188mAh·g-1、172mAh·g-1、152mAh·g-1。
Embodiment 3:Li1.1Mn0.2Co0.7O2Positive electrode
With Quilonorm (SKB), manganese acetate, cobalt acetate and oxalic acid for initiation material, 0.9804g manganese acetate, 3.4873g cobalt acetate, 2.4689g Quilonorm (SKB) are dissolved in dehydrated alcohol, obtain the metal salt solution of ethanol；Again the oxalic acid 6.3842g of than stoichiometric proportion excessive 20% is dissolved in dehydrated alcohol；The alcoholic solution of oxalic acid is added in the metal salt solution of ethanol, sucking filtration be ground into powder after 100 DEG C of dry 3h and load crucible after stirring 1h；It is warmed up at 900 DEG C with the programming rate of 4 DEG C/min in batch-type furnace and heats 12h, and in annealing at room temperature, Li can be obtained1.1Mn0.2Co0.7O2Powder body material.The XRD test result of powder body material shows, the powder body of synthesis has layered rock salt structure (R3m).The SEM test result of powder body material shows, the powder granule of synthesis is evenly distributed, and size is 300～500nm.Adopting button cell to test, the mass ratio of mixed powder, conductive carbon black and binding agent PVDF (Kynoar) is 8: 1: 1, and metal lithium sheet is to pole, 1mol L-1LiPF6/ EC+DMC+EMC (volume ratio 1: 1: 1) is electrolyte, and polypropylene material is barrier film, and battery test system is NEWARETC53, and charging/discharging voltage window is 2.0～4.6V, and charging and discharging currents density chooses 20mA g respectively-1、60mA·g-1、100mA·g-1、200mA·g-1, when this material is as the positive pole of lithium ion battery, show good chemical property.Button cell test result shows, (1) is at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and 28 DEG C at first discharge specific capacity respectively 219mAh g-1、206mAh·g-1、187mAh·g-1、168mAh·g-1；After 28 discharge and recharges, their specific discharge capacity respectively 188mAh g-1、177mAh·g-1、164mAh·g-1、147mAh·g-1.(2) at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and-10 DEG C at first discharge specific capacity respectively 176mAh g-1、159mAh·g-1、142mAh·g-1、118mAh·g-1, after 28 discharge and recharges, their specific discharge capacity respectively 168mAh g-1、149mAh·g-1、 131mAh·g-1、112mAh·g-1.(3) at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and 45.4 DEG C at first discharge specific capacity respectively 240mAh g-1、226mAh·g-1、201mAh·g-1、186mAh·g-1；After 28 discharge and recharges, their specific discharge capacity respectively 206mAh g-1、194mAh·g-1、176mAh·g-1、165mAh·g-1。
Embodiment 4:Li1.15Mn0.3Co0.55O2Positive electrode
With Quilonorm (SKB), manganese acetate, cobalt acetate and oxalic acid for initiation material, 1.4705g manganese acetate, 2.7400g cobalt acetate, 2.5811g Quilonorm (SKB) are dissolved in dehydrated alcohol, obtain the metal salt solution of ethanol；Again the oxalic acid 6.3993g of than stoichiometric proportion excessive 20% is dissolved in dehydrated alcohol；The alcoholic solution of oxalic acid is added in the metal salt solution of ethanol, sucking filtration be ground into powder after 100 DEG C of dry 3h and load crucible after stirring 1h；It is warmed up at 900 DEG C with the programming rate of 4 DEG C/min in batch-type furnace and heats 12h, and in annealing at room temperature, Li can be obtained1.15Mn0.3Co0.55O2Powder body material.The XRD test result of powder body material shows, the powder body of synthesis has layered rock salt structure (R3m).The SEM test result of powder body material shows, the powder granule of synthesis is evenly distributed, and size is 300～500nm.Adopting button cell to test, the mass ratio of mixed powder, conductive carbon black and binding agent PVDF (Kynoar) is 8: 1: 1, and metal lithium sheet is to pole, 1mol L-1LiPF6/ EC+DMC+EMC (volume ratio 1: 1: 1) is electrolyte, and polypropylene material is barrier film, and battery test system is NEWARETC53, and charging/discharging voltage window is 2.0～4.6V, and charging and discharging currents density chooses 20mA g respectively-1、60mA·g-1、100mA·g-1、200mA·g-1, when this material is as the positive pole of lithium ion battery, show good chemical property.Button cell test result shows, (1) is at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and 28 DEG C at first discharge specific capacity respectively 248mAh g-1、229mAh·g-1、206mAh·g-1、188mAh·g-1；After 28 discharge and recharges, their specific discharge capacity respectively 215mAh g-1、198mAh·g-1、181mAh·g-1、165mAh·g-1.(2) at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and-10 DEG C at first discharge specific capacity respectively 170mAh g-1、153mAh·g-1、139mAh·g-1、119mAh·g-1, after 28 discharge and recharges, their specific discharge capacity respectively 162mAh g-1、143mAh·g-1、128mAh·g-1、108mAh·g-1.(3) at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and 45.4 DEG C at first discharge specific capacity respectively 268mAh g-1、244mAh·g-1、217mAh·g-1、191mAh·g-1；After 28 discharge and recharges, their specific discharge capacity respectively 235mAh g-1、212mAh·g-1、193mAh·g-1、170mAh·g-1。
Embodiment 5:Li1.3Mn0.6Co0.1O2Positive electrode
With Quilonorm (SKB), manganese acetate, cobalt acetate and oxalic acid for initiation material, 2.9411g manganese acetate, 0.4982g cobalt acetate, 2.7851g Quilonorm (SKB) are dissolved in dehydrated alcohol, obtain the metal salt solution of ethanol；Again the oxalic acid 4.1830g of than stoichiometric proportion excessive 20% is dissolved in dehydrated alcohol；The alcoholic solution of oxalic acid is added in the metal salt solution of ethanol, sucking filtration be ground into powder after 100 DEG C of dry 3h and load crucible after stirring 1h；It is warmed up at 900 DEG C with the programming rate of 4 DEG C/min in batch-type furnace and heats 12h, and in annealing at room temperature, Li can be obtained1.3Mn0.6Co0.1O2Powder body material.The XRD test result of powder body material shows, the powder body of synthesis has layered rock salt structure (R3m).The SEM test result of powder body material shows, the powder granule of synthesis is evenly distributed, and size is 300～500nm.Adopting button cell to test, the mass ratio of mixed powder, conductive carbon black and binding agent PVDF (Kynoar) is 8: 1: 1, and metal lithium sheet is to pole, 1mol L-1LiPF6/ EC+DMC+EMC (volume ratio 1: 1: 1) is electrolyte, and polypropylene material is barrier film, and battery test system is NEWARETC53, and charging/discharging voltage window is 2.0～4.6V, and charging and discharging currents density chooses 20mA g respectively-1、60mA·g-1、100mA·g-1、200mA·g-1, when this material is as the positive pole of lithium ion battery, show good chemical property.Button cell test result shows, (1) is at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and 28 DEG C at first discharge specific capacity respectively 192mAh g-1、173mAh·g-1、155mAh·g-1、129mAh·g-1；After 28 discharge and recharges, their specific discharge capacity respectively 164mAh g-1、148mAh·g-1、140mAh·g-1、117mAh·g-1.(2) at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and-10 DEG C at first discharge specific capacity respectively 121mAh g-1、107mAh·g-1、96mAh·g-1、83mAh·g-1, after 28 discharge and recharges, their specific discharge capacity respectively 113mAh g-1、99mAh·g-1、86mAh·g-1、79mAh·g-1.(3) at 20mA g-1、60mA·g-1、100mA·g-1、200mA·g-1Charging and discharging currents density and 45.4 DEG C at first discharge specific capacity respectively 208mAh g-1、185mAh·g-1、174mAh·g-1、153mAh·g-1；After 28 discharge and recharges, their specific discharge capacity respectively 181mAh g-1、166mAh·g-1、154mAh·g-1、137mAh·g-1。
Claims (4)
1. a preparation method for lithium ion battery manganese cobalt lithium oxide anode material, comprises the steps:
(1) first weighing lithium salts, manganese salt and cobalt salt, the ratio making metal ion Li:Mn:Co is 1.033:0.067:0.9～1.3:0.6:0.1, the slaine weighed is dissolved in dehydrated alcohol, obtains alcoholic solution；
(2) weigh the oxalic acid measuring ratio little over quantification chemistry, and be dissolved in dehydrated alcohol, and add in the alcoholic solution that step (1) obtains, sucking filtration drying after stirring, obtain (LiMnCo)xC2O4Presoma；
(3) (LiMnCo) that step (2) is obtainedxC2O4After presoma carries out heat treatment and cooling process, it is thus achieved that Li(3+x)/3Mn2x/3Co1-xO2Positive electrode powder, wherein 0.1≤x≤0.9.
2. the preparation method of lithium ion battery manganese cobalt lithium oxide anode material according to claim 1, it is characterised in that: described lithium salts is one or more in Quilonorm (SKB), lithium nitrate, lithium chloride；Described manganese salt is one or more in manganese acetate, manganese nitrate, manganese chloride；Described cobalt salt is one or more in cobalt acetate, cobalt nitrate, cobaltous chloride.
3. the preparation method of lithium ion battery manganese cobalt lithium oxide anode material according to claim 1, it is characterised in that: described presoma is the coprecipitated thing of oxalates of lithium ion and transition metal ions, and mixing time is 0.5h～2h.
4. the preparation method of lithium ion battery manganese cobalt lithium oxide anode material according to claim 1, it is characterised in that: in described step (3), heat treatment temperature is 800 DEG C～1000 DEG C, time 3～16h；Cooling processing mode is quenching in quenching, mixture of ice and water in quenching, liquid nitrogen under room temperature.
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| CN102903909A (en) * | 2012-10-22 | 2013-01-30 | 中国科学院福建物质结构研究所 | Manganese-cobalt-lithium oxide positive electrode material of lithium ion battery and preparation method of material |
| CN103715411A (en) * | 2013-12-17 | 2014-04-09 | 中国科学院福建物质结构研究所 | Lithium ion battery manganese cobalt lithium oxide anode material and preparation method thereof |
| CN104201373A (en) * | 2014-08-22 | 2014-12-10 | 东莞市迈科科技有限公司 | Lithium-rich anode material and preparation method thereof |
| CN104201328A (en) * | 2014-08-22 | 2014-12-10 | 东莞市迈科科技有限公司 | High-capacity lithium anode material and preparation method thereof |
| CN104409685B (en) * | 2014-11-28 | 2017-09-22 | 东莞市迈科科技有限公司 | A kind of method for preparing the anode material for lithium-ion batteries with core shell structure |
| CN105958052A (en) * | 2016-05-29 | 2016-09-21 | 合肥国轩高科动力能源有限公司 | Preparation method for metal-element-doped manganese-based positive electrode material for lithium ion battery |
| CN106252650B (en) * | 2016-10-31 | 2018-11-13 | 安徽工业大学 | A kind of preparation method of stratiform lithium-rich manganese-based anode material |
| CN107768639A (en) * | 2017-10-19 | 2018-03-06 | 深圳市比克动力电池有限公司 | Anode material of lithium battery and preparation method thereof, the lithium battery using the positive electrode |
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