CN102013480A - Method for preparing laminated LiNi0.5Mn0.5O2 composite material as anode material of lithium ion battery - Google Patents
Method for preparing laminated LiNi0.5Mn0.5O2 composite material as anode material of lithium ion battery Download PDFInfo
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Abstract
The invention relates to a method for preparing LiNi0.5Mn0.5O2 as an anode material of a lithium ion battery, comprising the following steps of: completely dissolving soluble nickel salt and manganese salt in a molar ratio, drying to obtain a uniform precursor, and preburing; and fully grinding a lithium source compound and the precursor and calcining for 3-24 hours at 800-1000 DEG C in air to obtain uniformly doped LiNi0.5Mn0.5O2. The method is used for preparing the LiNi0.5Mn0.5O2 with single phase, stable structure and low ion disorder degree to obtain the anode material of the lithium ion battery, which has the advantages of large capacity, low internal resistance, high discharge time and good circulating performance. The electrode material can be applied to the actual lithium ion battery and has strong competitiveness at the aspects of discharge capacity, circulation, large-current discharge capacity and the like.
Description
Technical field
The present invention relates to the new forms of energy preparation field, be specifically related to a kind of anode material for lithium-ion batteries laminated Li-Ni-Mn-O compoiste material preparation method, particularly adopt solid phase method to prepare the method for Li-Ni-Mn-O compoiste material.
Background technology
In more than ten years in the past, lithium rechargeable battery has obtained sufficient research and has used widely, and increasing electronic device such as notebook computer, digital camera, MP5 etc. need lithium ion battery as long stabilized power supply.Along with non-renewable energy resources price such as oil in recent years rapidly increases, battery has many advantages as a kind of energy form.
Lithium ion battery development since coming out is compared advantage such as have the open circuit voltage height, energy density is big, memory-less effect, pollution-free and self discharge are little rapidly with secondary cells such as lead acid accumulator commonly used, nickel-cadmium cell, hydrogen nickel
[1], replace other secondary cells in various fields in a short period of time.Be widely used in fields such as portable Move tool, digital product, artificial satellite, Aero-Space at present, also had boundless prospect in fields such as electric bicycle and automobiles.Lithium ion battery also is considered to for electric bicycle, hybrid vehicle etc. provides the first-selection of clean energy resource at a low price, and this just requires this lithium ion battery not only to have high power capacity, also will have high-power simultaneously.Although Li
XC
6/ Li
1-XCoO
2Lithium ion battery can satisfy the requirement and the positive electrode LiFePO of most of mobile electronic product
4The demand of power source has been satisfied in existing improvement to a certain extent, but the Co resource-constrained, the cost height is harmful and the cobalt acid lithium battery fail safe is relatively poor relatively, LiFePO to environment
4Have the low defective of energy density that can't overcome and be not suitable for mobile electronic product, so people are seeking a kind of low cost, high-performance in recent years always, environmentally friendly and safe positive electrode replaces LiCoO
2
Stratiform Li-Ni-Mn-O is cheap, nontoxic, fail safe is good, is considered to promising replaceable commercialization LiCoO
2Anode material for lithium-ion batteries, LiNi wherein
0.5Mn
0.5O
2Be considered to the most potential material, because its theoretical capacity is 280mAh/g, Stability Analysis of Structures can not look like stratiform LiMnO in circulation simultaneously
2Equally change spinel structure into, low discharging current generally can reach the capacity of 200mAh/g at present.Although various synthetic methods are a lot of as solid phase method ([J] Y.Makimura et al Journal of Power Sources 2003 119-121 156-160 3, [J] K.Kang et al Science 2,006 311 977-980), coprecipitation ([J] Z.Lu et al Electrochemical and Solid-State Letters 2,001 4 A191-A194, [J] Z.Lu et al Journal of The Electrochemical Society 2,002 149 A778-A791), sol-gel process ([J] J.H.Kim et al Journal of Power Sources 2003 166-170 119-121), emulsification seasoning ([J] S.T.Myung et al Solid State Ionics 2,004 170 139-144), freeze-drying ([J] O.A.Shlyakhtin et al Electrochimica Acta 2,004 50 505-509), ultrasonic auxiliary law ([J] B.Zhang et al Solid State Ionics 2,007 178 1230-1234), hydro thermal method ([J] Cho.et al The Journal of Physical Chemistry C 2,007 111 3192-3196), ion-exchange ([J] K.Kang et al Science 2,006 311 977-980, [J] Y.Hinuma et al.Chemistry of Materials.2007 19 1790-1800) etc. is used to synthetic LiNi
0.5Mn
0.5O
2, but owing to exist dephasign and Li/Ni to arrange problems such as unordered in the crystal structure, be difficult to synthesize anode material for lithium-ion batteries LiNi with higher battery activity
0.5Mn
0.5O
2Addressing these problems topmost breakthrough recently has two, and one is by example switching method, Li
+Displacement Na
+Na (Ni
0.5Mn
0.5) O
2Be converted into Li (Ni
0.5Mn
0.5) O
2Another is to utilize the double-hydroxide coprecipitation of Ni and Mn promptly to measure than the Ni that is 1: 1 (OH)
2And Mn (OH)
2Solid solution is as predecessor.Preceding a kind of method is complicated multistep synthetic reaction, and needs to consume a large amount of lithium salts, and cost is difficult to control and complex operation, even if lithium salts is reclaimed, complexity is to a certain degree arranged also on the technology; A kind of method in back is then because Mn
2+In humid air, be easy to oxidizedly, need carefully controlled condition to obtain Ni (OH)
2And Mn (OH)
2Solid solution.So now the emphasis of research how also just to become can obtain uniform doping with a kind of straightforward procedure Ni, Mn solid solution as predecessor, finally prepare single-phase, Stability Analysis of Structures, LiNi that the ion degree of disorder is low
0.5Mn
0.5O
2Thereby, obtain big capacity, hang down the anode material for lithium-ion batteries of internal resistance, high-discharge-rate, good cycle.
Summary of the invention
The present invention will mainly utilize method simple and easy to control to obtain the effect that complex reaction could obtain, obtain the Ni, Mn solid solution of uniform doping as predecessor by simple solid reaction process, this predecessor is single-phase compound, the atom level Ni, the Mn that reach homogeneous mix, simultaneously not influenced by external condition, the present invention has overcome the limitation of prior art and has simplified complicated preparation process simultaneously.
Technical scheme of the present invention is as follows:
A kind of preparation method of laminated Li-Ni-Mn-O compoiste material is characterized in that: specifically comprise following step:
(1) take by weighing the nickel salt of solubility and the manganese salt of solubility respectively by stoichiometric proportion, put into the container that fills distilled water, and stir it is dissolved fully, make the liquid solution that drives of nickel salt and manganese salt, wherein the mol ratio of nickel and manganese is 1: (1-1.02);
(2) evaporate to dryness nickel salt and manganese salt precursor liquid solution obtain uniform nickel, manganese salt precipitation;
(3) will obtain uniform nickel, manganese salt precipitation and fully grind after, thereby in air atmosphere 800-1000 ℃ down calcining obtained the single-phase predecessor of uniform doping in 6-12 hour;
(4) single-phase predecessor and the lithium salts that (3) are obtained fully mixes according to certain ratio, ball milling, heating rate with 1-10 ℃/min divides two-section calcining to obtain laminated Li-Ni-Mn-O compoiste material, and wherein the mol ratio of Li and presoma is (1-1.03): 1, and the concrete steps of double sintering are as follows:
A, the mixture of predecessor and lithium salts is placed box type furnace, at 400-600 ℃ of heating 2-5h down;
B, with (1) heating after mixture ball milling 1-4h;
C, the material behind the ball milling is placed box type furnace, at 800-1000 ℃ of heating 3-24h down;
D, grinding obtain the end product laminated Li-Ni-Mn-O compoiste material after sieving.
The preparation method of described laminated Li-Ni-Mn-O compoiste material is characterized in that: described water-soluble nickel salt is selected from a kind of in nickel nitrate, nickel hydroxide, nickelous sulfate, the nickel acetate; Described water-soluble manganese salt is selected from a kind of in manganese nitrate, manganous hydroxide, manganese carbonate, the manganese acetate.
The preparation method of described laminated Li-Ni-Mn-O compoiste material is characterized in that: described lithium salts is selected from a kind of in lithium hydroxide, lithium acetate, lithium carbonate, the lithium nitrate.
Stratiform LiNi of the present invention
0.5Mn
0.5O
2The electrical property of composite material adopts two electrode simulated batteries, positive electrode active material powder, conductive agent acetylene black, adhesive PVDF, it by mass ratio 75: 20: 5 mixed, negative pole is a metal lithium sheet, and barrier film is the Celgard2400 microporous barrier, and electrolyte is 1MLiPF
6/ EC+EMC+DEC (volume ratio 1: 1: 1).
Advantage of the present invention is
(1) handles presoma by straightforward procedure, obtain the molecule level mixture, finally prepare single-phase, Stability Analysis of Structures, LiNi that the ion degree of disorder is low
0.5Mn
0.5O
2, optimized the physical and chemical performance of material.
(2) have higher battery activity, thereby obtain the anode material for lithium-ion batteries of big capacity, low internal resistance, high-discharge-rate, good cycle.And the kind electrode material has the value of application in the lithium ion battery of reality, reaches the purpose of upgrading electrode material.
Description of drawings
Fig. 1 is the Ni of solid phase synthesis preparation of the present invention
1.5Mn
1.5O
4The XRD figure of presoma.
Fig. 2 is the SEM figure of presoma.
Fig. 3 is embodiment 1 stratiform LiNi
0.5Mn
0.5O
2XRD figure.
Fig. 4 is that embodiment 1 is with 0.1C multiplying power first charge-discharge curve.
Fig. 5 is that embodiment 1 is with 0.2C, 0.5C, 1C, 2C, 5C multiplying power discharging curve.
Fig. 6 is embodiment 1 with the cycle performance figure of 1C multiplying power discharging 150 times.
Embodiment:
Embodiment 1
24.89g nickel acetate, 11.50 manganese carbonates of stoichiometric proportion are dissolved in the distilled water fully, thereby with dried uniform nickel, the manganese salt precipitation of obtaining of solution evaporation.Thereby in air atmosphere, calcine under 800 ℃ after fully grinding and obtained the single-phase predecessor of uniform doping in 12 hours.
Predecessor and lithium acetate 20.40g according to abundant mixed grinding, be warmed up to 500 ℃ of constant temperature 3 hours in air atmosphere with the programming rate of 5 ℃/min, cooling is fully ground the back and is warmed up to 900 ℃ with the programming rate of 5C/min and calcines in air atmosphere, obtains end product LiNi thereby calcination time is 6h
0.5Mn
0.5O
2Electrochemical property test is seen Fig. 4, Fig. 5, Fig. 6.
29.08g nickel nitrate, the 40.01g manganese nitrate of stoichiometric proportion are dissolved in the distilled water, solution is evaporated dried uniform nickel, the manganese salt precipitation of obtaining.Thereby in air atmosphere, calcine under 600-800 ℃ after fully grinding and obtained the single-phase predecessor of uniform doping in 12 hours.Through XRD, ICP, SEM test, show to consist of Ni
1.5Mn
1.5O
4, belong to the Fd3m space group, have cubic structure.
Predecessor and the abundant mixed grinding of lithium hydroxide 8.392g, be warmed up to 500 ℃ of constant temperature 3 hours in air atmosphere with the programming rate of 5 ℃/min, cooling is fully ground the back and is warmed up to 800 ℃-900 ℃ with the programming rate of 5 ℃/min and calcines in air atmosphere, obtains end product LiNi thereby calcination time is 6h
0.5Mn
0.5O
2Test result sees the following form:
The experimental result of table 1 embodiment 2
| Calcining heat | Discharge capacity first | The initial charge capacity | First charge-discharge efficiency % |
| 800℃ | 178.1 | 200.9 | 88.7 |
| 850℃ | 199.8 | 207.3 | 96.3 |
| 900℃ | 189.9 | 210.7 | 90.1 |
Embodiment 3
Nickel hydroxide 9.271g, the manganese nitrate 11.50g of stoichiometric proportion are dissolved in the distilled water, solution is evaporated dried uniform nickel, the manganese salt precipitation of obtaining.Thereby in air atmosphere, calcine under 800 ℃ after fully grinding and obtained the single-phase predecessor of uniform doping in 12 hours.Through XRD, ICP, SEM test, show to consist of Ni
1.5Mn
1.5O
4, belong to the Fd3m space group, have cubic structure.
Predecessor and the abundant mixed grinding of lithium nitrate 13.79g, be warmed up to 500 ℃ of constant temperature 3 hours in air atmosphere with the programming rate of 5 ℃/min, cooling is fully ground the back and is warmed up to 800 ℃-900 ℃ with the programming rate of 5 ℃/min and calcines in air atmosphere, obtains end product LiNi thereby calcination time is 3-24h
0.5Mn
0.5O
2Test result sees the following form:
The LiNi that table 2 embodiment prepares for 3 times
0.5Mn
0.5O
2Chemical property (unit: mAh/g)
| Calcination time | Discharge capacity first | The initial charge capacity | First charge-discharge efficiency % |
| 3h | 181.1 | 209.9 | 86.3 |
| 6h | 187.3 | 204.6 | 91.5 |
| 12h | 199.8 | 207.3 | 96.3 |
| 24h | 190.4 | 204.0 | 93.3 |
Embodiment 4
Nickel acetate 24.89g, the manganese acetate 24.51g of stoichiometric proportion are dissolved in the distilled water, solution is evaporated dried uniform nickel, the manganese salt precipitation of obtaining.Thereby in air atmosphere, calcine under 800 ℃ after fully grinding and obtained the single-phase predecessor of uniform doping in 12 hours.Through XRD, ICP, SEM test, show to consist of Ni
1.5Mn
1.5O
4, belong to the Fd3m space group, have cubic structure.
Predecessor and the abundant mixed grinding of lithium carbonate 7.38g, be warmed up to 500 ℃ of constant temperature 3 hours in air atmosphere with the programming rate of 1-10 ℃/min, cooling is fully ground the back and is warmed up to 800 ℃-900 ℃ with the programming rate of 1-10 ℃/min and calcines in air atmosphere, obtains end product LiNi thereby calcination time is 12h
0.5Mn
0.5O
2Test result sees the following form:
The LiNi that table 3 embodiment 3 prepares
0.5Mn
0.5O
2Chemical property (unit: mAh/g)
| Heating rate | Discharge capacity first | The initial charge capacity | First charge-discharge efficiency % |
| 1℃/min | 174.5 | 205.1 | 85.1 |
| 2℃/min | 191.8 | 201.2 | 95.3 |
| 5℃/min | 199.8 | 207.4 | 96.3 |
| 10℃/min | 179.2 | 207.2 | 86.5 |
Embodiment 5
Nickel acetate 24.89g, the manganese acetate 24.51g of stoichiometric proportion are dissolved in the distilled water, solution is evaporated dried uniform nickel, the manganese salt precipitation of obtaining.Thereby in air atmosphere, calcine under 800 ℃ after fully grinding and obtained the single-phase predecessor of uniform doping in 12 hours.Through XRD, ICP, SEM test, show to consist of Ni
1.5Mn
1.5O
4, belong to the Fd3m space group, have cubic structure.
The abundant mixed grinding of predecessor and 1: 1 (13.79g), 1: 1.01 (13.93g) of lithium nitrate, 1: 1.02 (14.07g), 1: 1.03 (14.20g), be warmed up to 500 ℃ of constant temperature 3 hours in air atmosphere with the programming rate of 5C/min, cooling is fully ground the back and is warmed up to 800 ℃-900 ℃ with the programming rate of 5 ℃/min and calcines in air atmosphere, obtains end product LiNi thereby calcination time is 12h
0.5Mn
0.5O
2Test result sees the following form:
The LiNi that table 4 embodiment 3 prepares
0.5Mn
0.5O
2Chemical property (unit: mAh/g)
| Heating rate | Discharge capacity first | The initial charge capacity | First charge-discharge efficiency % |
| 1∶1 | 182.6 | 199.7 | 91.4 |
| 1∶1.01 | 185.4 | 200.5 | 92.5 |
| 1∶1.02 | 190.3 | 204.4 | 93.1 |
| 1∶1.03 | 187.8 | 203.2 | 92.4 |
Claims (3)
1. the preparation method of a laminated Li-Ni-Mn-O compoiste material is characterized in that: specifically comprise following step:
(1) take by weighing the nickel salt of solubility and the manganese salt of solubility respectively by stoichiometric proportion, put into the container that fills distilled water, and stir it is dissolved fully, make the liquid solution that drives of nickel salt and manganese salt, wherein the mol ratio of nickel and manganese is 1: (1-1.02);
(2) evaporate to dryness nickel salt and manganese salt precursor liquid solution obtain uniform nickel, manganese salt precipitation;
(3) will obtain uniform nickel, manganese salt precipitation and fully grind after, thereby in air atmosphere 800-1000 ℃ down calcining obtained the single-phase predecessor of uniform doping in 6-12 hour;
(4) single-phase predecessor and the lithium salts that (3) are obtained fully mixes according to certain ratio, ball milling, heating rate with 1-10 ℃/min divides two-section calcining to obtain laminated Li-Ni-Mn-O compoiste material, and wherein the mol ratio of Li and presoma is (1-1.03): 1, and the concrete steps of double sintering are as follows:
A, the mixture of predecessor and lithium salts is placed box type furnace, at 400-600 ℃ of heating 2-5h down;
B, with (1) heating after mixture ball milling 1-4h;
C, the material behind the ball milling is placed box type furnace, at 800-1000 ℃ of heating 3-24h down;
D, grinding obtain the end product laminated Li-Ni-Mn-O compoiste material after sieving.
2. according to the preparation method of right 1 described laminated Li-Ni-Mn-O compoiste material, it is characterized in that: described water-soluble nickel salt is selected from a kind of in nickel nitrate, nickel hydroxide, nickelous sulfate, the nickel acetate; Described water-soluble manganese salt is selected from a kind of in manganese nitrate, manganous hydroxide, manganese carbonate, the manganese acetate.
3. the preparation method of laminated Li-Ni-Mn-O compoiste material according to claim 1 is characterized in that: described lithium salts is selected from a kind of in lithium hydroxide, lithium acetate, lithium carbonate, the lithium nitrate.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102324512A (en) * | 2011-09-19 | 2012-01-18 | 奇瑞汽车股份有限公司 | Surface-coated high voltage anode material LiNi0.5Mn1.5O4 and preparation method thereof |
| CN102569776A (en) * | 2011-12-30 | 2012-07-11 | 合肥国轩高科动力能源有限公司 | Preparation method of spinel type lithium manganese oxide for spherical high-voltage anode material |
| CN102664250A (en) * | 2012-05-09 | 2012-09-12 | 奇瑞汽车股份有限公司 | Lithium nickel manganese oxygen material and preparation method thereof and lithium ion battery containing lithium nickel manganese oxygen material |
| CN103606673A (en) * | 2013-11-14 | 2014-02-26 | 江苏大学 | Preparation method of laminar-spinel compound sosoloid anode material |
| CN103972495A (en) * | 2014-05-16 | 2014-08-06 | 盐城市新能源化学储能与动力电源研究中心 | Preparation method of lithium ion battery positive pole material lithium nickelate manganate |
| CN110098405A (en) * | 2019-03-22 | 2019-08-06 | 长沙理工大学 | A kind of preparation method of anode material for lithium ion battery |
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| CN1688045A (en) * | 2005-03-18 | 2005-10-26 | 上海瀛正科技有限公司 | Method for preparing laminated Li-Ni-Mn-O compoiste material and its application |
| CN1960035A (en) * | 2006-11-06 | 2007-05-09 | 北京科技大学 | Method for preparing laminar Li [Ni1/2Mn1/2]O2 material in use for lithium ion battery |
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2010
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102324512A (en) * | 2011-09-19 | 2012-01-18 | 奇瑞汽车股份有限公司 | Surface-coated high voltage anode material LiNi0.5Mn1.5O4 and preparation method thereof |
| CN102569776A (en) * | 2011-12-30 | 2012-07-11 | 合肥国轩高科动力能源有限公司 | Preparation method of spinel type lithium manganese oxide for spherical high-voltage anode material |
| CN102569776B (en) * | 2011-12-30 | 2014-07-02 | 合肥国轩高科动力能源股份公司 | Preparation method of spinel type lithium manganese oxide for spherical high-voltage anode material |
| CN102664250A (en) * | 2012-05-09 | 2012-09-12 | 奇瑞汽车股份有限公司 | Lithium nickel manganese oxygen material and preparation method thereof and lithium ion battery containing lithium nickel manganese oxygen material |
| CN103606673A (en) * | 2013-11-14 | 2014-02-26 | 江苏大学 | Preparation method of laminar-spinel compound sosoloid anode material |
| CN103606673B (en) * | 2013-11-14 | 2016-07-20 | 江苏大学 | A kind of preparation method of laminar-spinel compound sosoloid anode material |
| CN103972495A (en) * | 2014-05-16 | 2014-08-06 | 盐城市新能源化学储能与动力电源研究中心 | Preparation method of lithium ion battery positive pole material lithium nickelate manganate |
| CN103972495B (en) * | 2014-05-16 | 2016-03-23 | 盐城市新能源化学储能与动力电源研究中心 | A kind of preparation method of lithium ion battery anode material nickel LiMn2O4 |
| CN110098405A (en) * | 2019-03-22 | 2019-08-06 | 长沙理工大学 | A kind of preparation method of anode material for lithium ion battery |
| CN110098405B (en) * | 2019-03-22 | 2022-06-10 | 长沙理工大学 | Preparation method of anode material for lithium ion battery |
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Application publication date: 20110413 |