CN102751483A - Layered rich-lithium-manganese-based solid-solution anode material of lithium ion battery and method for preparing anode material - Google Patents
Layered rich-lithium-manganese-based solid-solution anode material of lithium ion battery and method for preparing anode material Download PDFInfo
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- CN102751483A CN102751483A CN2012102495086A CN201210249508A CN102751483A CN 102751483 A CN102751483 A CN 102751483A CN 2012102495086 A CN2012102495086 A CN 2012102495086A CN 201210249508 A CN201210249508 A CN 201210249508A CN 102751483 A CN102751483 A CN 102751483A
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Abstract
The invention discloses a method for preparing a layered rich-lithium-manganese-based solid-solution anode material of a lithium ion battery. The chemical formula of the anode material is xLi2MnO3*(1-x) Li Mn 0.4Ni0.4NCo0.2O2 (x=0.1-1.0). The anode material is prepared by methods of heat treatment and cooling treatment for a precursor. The anode material prepared by the method has excellent electrochemistry performances such as high specific capacity and good circulation performance.
Description
Technical field
The present invention relates to the lithium-rich manganese-based solid solution method for preparing anode material of a kind of lithium ion battery stratiform in the lithium ion battery field.
Background technology
Advantages such as lithium ion battery has that voltage height, volume are little, light weight, specific energy are big, have extended cycle life, security performance is good; Be widely used in the electronic equipments such as video camera, mobile phone, notebook computer and Portable Measurement Instrument, and in fields such as electric automobile, space technology, had broad application prospects.At present, the preparation of lithium-rich manganese-based solid-solution material great majority adopt coprecipitation, and technologies such as part bibliographical information sol-gal process, solid phase method, ion-exchange and firing method are also arranged.Though coprecipitation is used extensively, the adjusting of its technological parameter and control difficulty; Sol-gal process need consume lot of organic acids or alcohol raises cost; Ion-exchange and firing method technology are loaded down with trivial details, are not suitable for large-scale production; Traditional solid sintering technology batch mixing uniformity material repeatability relatively poor, preparation is relatively poor.The present invention adopts a kind of low temperature solid sintering technology to prepare the lithium-rich manganese-based solid solution positive electrode of lithium ion battery stratiform, and this method technical process is simple, is easy to control, good reproducibility, and cost is low, and excellent product performance, has the heavy industrialization application prospect.
Summary of the invention
The object of the present invention is to provide the lithium-rich manganese-based solid solution method for preparing anode material of a kind of lithium ion battery stratiform, the chemical formula of this positive electrode can be expressed as: xLi
2MnO
3(1-x) LiMn
0.4Ni
0.4Co
0.2O
2(x=0.1～1.0).
The positive electrode of the lithium-rich manganese-based solid solution lithium ion battery of stratiform of method preparation provided by the present invention not only has higher specific capacity performance, and has excellent cycle performance.
The preparation method of the lithium-rich manganese-based solid solution positive electrode of stratiform provided by the invention may further comprise the steps:
(1) at first according to composite material xLi
2MnO
3(1-x) LiMn
0.4Ni
0.4Co
0.2O
2The composition of (x=0.1～1.0) takes by weighing a certain amount of lithium salts, manganese salt, nickel salt and cobalt salt according to stoichiometric proportion, and the raw material ground and mixed is even;
(2) take by weighing the oxalic acid that is in excess in stoichiometric proportion slightly, add step (1) gained mixture and grind or ball milling, dried obtains rice white bulk (LiMnNiCo)
xC
2O
4Presoma;
(3) (LiMnNiCo) that step (2) is obtained
xC
2O
4Presoma carries out Low Temperature Heat Treatment, high-temperature heat treatment and cooling processing after grinding fully, obtains xLi
2MnO
3(1-x) LiMn
0.4Ni
0.4Co
0.2O
2Solid solution class composite positive pole.
Lithium salts in the above-mentioned steps (1) is one or more in lithium acetate, lithium nitrate, the lithium chloride; Manganese salt is one or more in manganese acetate, manganese nitrate, the manganese chloride; Cobalt salt is one or more in cobalt acetate, cobalt nitrate, the cobalt chloride; Nickel salt is one or more in nickel acetate, nickel nitrate, the nickel chloride;
The time of grinding or ball-milling treatment is 2～10h in the step (2); The temperature of dried is 80 ℃～150 ℃, and the processing time is 6～15h;
The Low Temperature Heat Treatment temperature is 300 ℃～450 ℃ in the step (3), time 2～8h, and the high-temperature heat treatment temperature is 800 ℃～1000 ℃, time 8 ~ 20h; The cooling processing mode is to quench in quenching, the mixture of ice and water in quenching, the liquid nitrogen under the room temperature.
The present invention adopts low-temperature solid-phase method to prepare xLi
2MnO
3(1-x) LiMn
0.4Ni
0.4Co
0.2O
2Positive electrode; Utilize slaine and oxalic acid at room temperature to react; Lithium ion and even mix of other transition metal ionss on molecular level have been realized; Solved lithium ion in the coprecipitation and failed to form the problem of common hypostasis, overcome traditional uneven difficulty of solid phase method raw materials mix simultaneously, improved the degree that is uniformly dispersed and the homogeneity of product greatly with transition metal ions; The method that the present invention adopts is not introduced foreign ion, has improved product gas purity to a great extent, has solved the problem that foreign ion works the mischief to material property; In addition, the method that the present invention takes, technology is simple, easy to operate, has shortened processing step greatly, has practiced thrift ample resources, helps sequencing production, has practiced thrift production cost.The raw material sources that the present invention adopts are extensive, and process equipment is simple, are easy to control, and good reproducibility can synthesize in scale.The synthetic method that the present invention adopts is not limited to the material that the present invention announces, can also be used for the synthetic of other materials, and this method has broad application prospects.
Description of drawings
Fig. 1 is embodiment 1 0.3Li
2MnO
30.7LiMn
0.4Ni
0.4Co
0.2O
2The X-ray diffracting spectrum of positive electrode powder.
Fig. 2 uses 0.3Li for embodiment 1
2MnO
30.7LiMn
0.4Ni
0.4Co
0.2O
2The positive electrode powder is as positive pole 20mAg at room temperature
-1, 50mAg
-1, 100mAg
-1, 200mAg
-1The time charging and discharging curve.
Fig. 3 uses 0.3Li for embodiment 1
2MnO
30.7LiMn
0.4Ni
0.4Co
0.2O
2The positive electrode powder is as positive pole 20mAg at room temperature
-1, 50mAg
-1, 100mAg
-1, 200mAg
-1The time the cycle performance curve.
Embodiment
Main implementation process of the present invention is:
(1) at first according to composite material xLi
2MnO
3(1-x) LiMn
0.4Ni
0.4Co
0.2O
2The composition of (x=0.1～1.0) takes by weighing a certain amount of lithium salts, manganese salt, nickel salt and cobalt salt according to stoichiometric proportion, and the raw material ground and mixed is even;
(2) take by weighing the oxalic acid that is in excess in stoichiometric proportion slightly, add step (1) gained mixture and grind or ball milling, dried obtains rice white bulk (LiMnNiCo)
xC
2O
4Presoma;
(3) (LiMnNiCo) that step (2) is obtained
xC
2O
4Presoma carries out Low Temperature Heat Treatment, high-temperature heat treatment and cooling processing after grinding fully, obtains xLi
2MnO
3(1-x) LiMn
0.4Ni
0.4Co
0.2O
2Solid solution class composite positive pole.
Below further illustrate characteristics of the present invention through instance, but be not limited to embodiment.
Experimental technique among the following embodiment if no special instructions, is conventional method.
Embodiment 1:0.3Li
2MnO
30.7LiMn
0.4Ni
0.4Co
0.2O
2Positive electrode
With lithium acetate, manganese acetate, nickel acetate, cobalt acetate and oxalic acid are initiation material, take by weighing 2.8431g manganese acetate, 1.3941g nickel acetate, 0.6977g cobalt acetate, 2.9183g lithium acetate and 5.1895g oxalic acid.The mixed material that takes by weighing fully ground behind 80 ℃ of oven drying 12h, be ground into the powder crucible of packing into behind the 2h; Programming rate with 4 ℃/min in box type furnace is warmed up to 350 ℃ of heating 3h down, and the programming rate with 4 ℃/min is warmed up to 900 ℃ of heating 16h down again, and under room temperature, quenches, and can obtain 0.3Li
2MnO
30.7LiMn
0.4Ni
0.4Co
0.2O
2Powder body material.The XRD test result of powder body material shows that synthetic powder has stratiform rock salt structure (R3m), and is as shown in Figure 1.Adopt 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 the utmost point, 1molL
-1LiPF
6/ EC+DMC+EMC (volume ratio 1:1:1) is an electrolyte, and polypropylene material is a barrier film, and battery test system is NEWARE TC53, and the charging/discharging voltage window is 2.0～4.8V, and charging and discharging currents density is chosen 20mAg respectively
-1, 50mAg
-1, 100mAg
-1, 200mAg
-1, this material shows good electrochemical during as lithium ion battery anodal.The button cell test result shows, at 20mAg
-1, 50mAg
-1, 100mAg
-1, 200mAg
-1Charging and discharging currents density and 28 ℃ of following first discharge specific capacity be respectively 253mAhg
-1, 232mAhg
-1, 189mAhg
-1, 158mAhg
-1, as shown in Figure 2; After discharging and recharging through 30 times, their specific discharge capacity is respectively 222mAhg
-1, 207mAhg
-1, 163mAhg
-1, 145mAhg
-1, as shown in Figure 3.
Embodiment 2:0.4Li
2MnO
30.6LiMn
0.4Ni
0.4Co
0.2O
2Positive electrode
With lithium acetate, manganese acetate, nickel acetate, cobalt acetate and oxalic acid are initiation material, take by weighing 3.1372g manganese acetate, 1.1944g nickel acetate, 0.5978g cobalt acetate, 3.1422g lithium acetate and 5.3555g oxalic acid.The mixed material that takes by weighing fully ground behind 80 ℃ of oven drying 12h, be ground into the powder crucible of packing into behind the 2h; Programming rate with 4 ℃/min in box type furnace is warmed up to 350 ℃ of heating 3h down, and the programming rate with 4 ℃/min is warmed up to 900 ℃ of heating 16h down again, and under room temperature, quenches, and can obtain 0.4Li
2MnO
30.6LiMn
0.4Ni
0.4Co
0.2O
2Powder body material.The XRD test result of powder body material shows that synthetic powder has stratiform rock salt structure (R3m).Adopt 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 the utmost point, 1molL
-1LiPF
6/ EC+DMC+EMC (volume ratio 1:1:1) is an electrolyte, and polypropylene material is a barrier film, and battery test system is NEWARE TC53, and the charging/discharging voltage window is 2.0～4.8V, and charging and discharging currents density is chosen 20mAg respectively
-1, 50mAg
-1, 100mAg
-1, 200mAg
-1, this material shows good electrochemical during as lithium ion battery anodal.The button cell test result shows, at 20mAg
-1, 50mAg
-1, 100mAg
-1, 200mAg
-1Charging and discharging currents density and 28 ℃ of following first discharge specific capacity be respectively 234mAhg
-1, 201mAhg
-1, 169mAhg
-1, 137mAhg
-1After discharging and recharging through 30 times, their specific discharge capacity is respectively 201mAhg
-1, 185mAhg
-1, 150mAhg
-1, 120mAhg
-1
Embodiment 3:0.5Li
2MnO
30.5LiMn
0.4Ni
0.4Co
0.2O
2Positive electrode
With lithium acetate, manganese acetate, nickel acetate, cobalt acetate and oxalic acid are initiation material, take by weighing 3.4313g manganese acetate, 0.9954g nickel acetate, 0.4982g cobalt acetate, 3.3667g lithium acetate and 5.5219g oxalic acid.The mixed material that takes by weighing fully ground behind 80 ℃ of oven drying 12h, be ground into the powder crucible of packing into behind the 2h; Programming rate with 4 ℃/min in box type furnace is warmed up to 350 ℃ of heating 3h down, and the programming rate with 4 ℃/min is warmed up to 900 ℃ of heating 16h down again, and under room temperature, quenches, and can obtain 0.5Li
2MnO
30.5LiMn
0.4Ni
0.4Co
0.2O
2Powder body material.The XRD test result of powder body material shows that synthetic powder has stratiform rock salt structure (R3m).Adopt 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 the utmost point, 1molL
-1LiPF
6/ EC+DMC+EMC (volume ratio 1:1:1) is an electrolyte, and polypropylene material is a barrier film, and battery test system is NEWARE TC53, and the charging/discharging voltage window is 2.0～4.8V, and charging and discharging currents density is chosen 20mAg respectively
-1, 50mAg
-1, 100mAg
-1, 200mAg
-1, this material shows good electrochemical during as lithium ion battery anodal.The button cell test result shows, at 20mAg
-1, 50mAg
-1, 100mAg
-1, 200mAg
-1Charging and discharging currents density and 28 ℃ of following first discharge specific capacity be respectively 230mAhg
-1, 205mAhg
-1, 173mAhg
-1, 145mAhg
-1After discharging and recharging through 30 times, their specific discharge capacity is respectively 199mAhg
-1, 187mAhg
-1, 152mAhg
-1, 123mAhg
-1
Embodiment 4:0.1Li
2MnO
30.9LiMn
0.4Ni
0.4Co
0.2O
2Positive electrode
With lithium acetate, manganese acetate, nickel acetate, cobalt acetate and oxalic acid are initiation material, take by weighing 2.2548g manganese acetate, 1.7916g nickel acetate, 0.8967g cobalt acetate, 2.4689g lithium acetate and 4.8562g oxalic acid.The mixed material that takes by weighing fully ground behind 80 ℃ of oven drying 12h, be ground into the powder crucible of packing into behind the 2h; Programming rate with 4 ℃/min in box type furnace is warmed up to 350 ℃ of heating 3h down, and the programming rate with 4 ℃/min is warmed up to 900 ℃ of heating 16h down again, and under room temperature, quenches, and can obtain 0.1Li
2MnO
30.9LiMn
0.4Ni
0.4Co
0.2O
2Powder body material.The XRD test result of powder body material shows that synthetic powder has stratiform rock salt structure (R3m).Adopt 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 the utmost point, 1molL
-1LiPF
6/ EC+DMC+EMC (volume ratio 1:1:1) is an electrolyte, and polypropylene material is a barrier film, and battery test system is NEWARE TC53, and the charging/discharging voltage window is 2.0～4.8V, and charging and discharging currents density is chosen 20mAg respectively
-1, 50mAg
-1, 100mAg
-1, 200mAg
-1, this material shows good electrochemical during as lithium ion battery anodal.The button cell test result shows, at 20mAg
-1, 50mAg
-1, 100mAg
-1, 200mAg
-1Charging and discharging currents density and 28 ℃ of following first discharge specific capacity be respectively 233mAhg
-1, 209mAhg
-1, 197mAhg
-1, 185mAhg
-1After discharging and recharging through 30 times, their specific discharge capacity is respectively 195mAhg
-1, 189mAhg
-1, 177mAhg
-1, 168mAhg
-1
Embodiment 5:0.2Li
2MnO
30.8LiMn
0.4Ni
0.4Co
0.2O
2Positive electrode
With lithium acetate, manganese acetate, nickel acetate, cobalt acetate and oxalic acid are initiation material, take by weighing 2.5489g manganese acetate, 1.5926g nickel acetate, 0.7971g cobalt acetate, 2.6933g lithium acetate and 5.0226g oxalic acid.The mixed material that takes by weighing fully ground behind 80 ℃ of oven drying 12h, be ground into the powder crucible of packing into behind the 2h; Programming rate with 4 ℃/min in box type furnace is warmed up to 350 ℃ of heating 3h down, and the programming rate with 4 ℃/min is warmed up to 900 ℃ of heating 16h down again, and under room temperature, quenches, and can obtain 0.2Li
2MnO
30.8LiMn
0.4Ni
0.4Co
0.2O
2Powder body material.The XRD test result of powder body material shows that synthetic powder has stratiform rock salt structure (R3m).Adopt 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 the utmost point, 1molL
-1LiPF
6/ EC+DMC+EMC (volume ratio 1:1:1) is an electrolyte, and polypropylene material is a barrier film, and battery test system is NEWARE TC53, and the charging/discharging voltage window is 2.0～4.8V, and charging and discharging currents density is chosen 20mAg respectively
-1, 50mAg
-1, 100mAg
-1, 200mAg
-1, this material shows good electrochemical during as lithium ion battery anodal.The button cell test result shows, at 20mAg
-1, 50mAg
-1, 100mAg
-1, 200mAg
-1Charging and discharging currents density and 28 ℃ of following first discharge specific capacity be respectively 245mAhg
-1, 208mAhg
-1, 197mAhg
-1, 180mAhg
-1After discharging and recharging through 30 times, their specific discharge capacity is respectively 223mAhg
-1, 191mAhg
-1, 181mAhg
-1, 167mAhg
-1
Claims (5)
1. the lithium-rich manganese-based solid solution positive electrode of lithium ion battery stratiform, the chemical formula of this positive electrode can be expressed as: xLi
2MnO
3(1-x) LiMn
0.4Ni
0.4Co
0.2O
2(x=0.1～1.0).
2. the preparation method of the described positive electrode of claim 1 comprises the steps:
(1) at first according to composite material xLi
2MnO
3(1-x) LiMn
0.4Ni
0.4Co
0.2O
2The composition of (x=0.1～1.0) takes by weighing a certain amount of lithium salts, manganese salt, nickel salt and cobalt salt according to stoichiometric proportion, and the raw material ground and mixed is even;
(2) take by weighing the oxalic acid that is in excess in stoichiometric proportion slightly, add step (1) gained mixture and grind or ball milling, dried obtains rice white bulk (LiMnNiCo)
xC
2O
4Presoma;
(3) (LiMnNiCo) that step (2) is obtained
xC
2O
4Presoma carries out Low Temperature Heat Treatment, high-temperature heat treatment and cooling processing after grinding fully, obtains xLi
2MnO
3(1-x) LiMn
0.4Ni
0.4Co
0.2O
2Solid solution class composite positive pole.
3. the preparation method of positive electrode according to claim 2, it is characterized in that: the lithium salts in the said step (1) is one or more in lithium acetate, lithium nitrate, the lithium chloride; Manganese salt is one or more in manganese acetate, manganese nitrate, the manganese chloride; Cobalt salt is one or more in cobalt acetate, cobalt nitrate, the cobalt chloride; Nickel salt is one or more in nickel acetate, nickel nitrate, the nickel chloride.
4. the preparation method of positive electrode according to claim 2 is characterized in that: grind in the said step (2) or the time of ball-milling treatment is 2～10h; The temperature of dried is 80 ℃～150 ℃, and the processing time is 6～15h.
5. the preparation method of positive electrode according to claim 2 is characterized in that: the Low Temperature Heat Treatment temperature is 300 ℃～450 ℃ in the said step (3), time 2～8h, and the high-temperature heat treatment temperature is 800 ℃～1000 ℃, time 8 ~ 20h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102916176A (en) * | 2012-11-02 | 2013-02-06 | 多氟多化工股份有限公司 | Microsphere laminated lithium-enriched manganese-based solid solution anode material and preparation method thereof |
| CN103468211A (en) * | 2013-09-25 | 2013-12-25 | 深圳市旭冉电子有限公司 | Abrasive and coating slurry of lithium-ion power battery diaphragm and preparation methods thereof |
| CN107104245A (en) * | 2017-05-03 | 2017-08-29 | 南京安普瑞斯有限公司 | A kind of lithium ion battery |
| CN109148879A (en) * | 2018-09-30 | 2019-01-04 | 桑顿新能源科技有限公司 | A kind of preparation method of lithium ion battery lithium-rich manganese-based anode material |
| CN109546115A (en) * | 2018-11-19 | 2019-03-29 | 安徽安凯汽车股份有限公司 | A kind of NCA ternary battery of nickelic rich lithium manganese base solid solution positive electrode |
| CN109860509A (en) * | 2019-01-14 | 2019-06-07 | 中国电力科学研究院有限公司 | A kind of preparation method of the rich lithium manganese base solid solution positive electrode of anion codope |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102916176A (en) * | 2012-11-02 | 2013-02-06 | 多氟多化工股份有限公司 | Microsphere laminated lithium-enriched manganese-based solid solution anode material and preparation method thereof |
| CN103468211A (en) * | 2013-09-25 | 2013-12-25 | 深圳市旭冉电子有限公司 | Abrasive and coating slurry of lithium-ion power battery diaphragm and preparation methods thereof |
| CN107104245A (en) * | 2017-05-03 | 2017-08-29 | 南京安普瑞斯有限公司 | A kind of lithium ion battery |
| CN109148879A (en) * | 2018-09-30 | 2019-01-04 | 桑顿新能源科技有限公司 | A kind of preparation method of lithium ion battery lithium-rich manganese-based anode material |
| CN109546115A (en) * | 2018-11-19 | 2019-03-29 | 安徽安凯汽车股份有限公司 | A kind of NCA ternary battery of nickelic rich lithium manganese base solid solution positive electrode |
| CN109860509A (en) * | 2019-01-14 | 2019-06-07 | 中国电力科学研究院有限公司 | A kind of preparation method of the rich lithium manganese base solid solution positive electrode of anion codope |
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