CN103579610A - Preparation method for lithium ion battery cathode material-lithium nickel manganese oxide - Google Patents
Preparation method for lithium ion battery cathode material-lithium nickel manganese oxide Download PDFInfo
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- CN103579610A CN103579610A CN201310586472.5A CN201310586472A CN103579610A CN 103579610 A CN103579610 A CN 103579610A CN 201310586472 A CN201310586472 A CN 201310586472A CN 103579610 A CN103579610 A CN 103579610A
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- Prior art keywords
- oxalate
- lithium
- nickel
- hydroxide
- manganese oxide
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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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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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
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a preparation method for a lithium ion battery cathode material-lithium nickel manganese oxide. The method adopts oxalate and hydroxide as precipitants at the same time for preparing lithium nickel manganese oxide through a coprecipitation method and a solid-phase sintering method. The method comprises the following steps: synthesizing a lithium nickel manganese oxide precursor by double precipitants, that is, synthesizing an oxalate/nickel hydroxide compound precursor material by controlling the pH value of a reaction solution according to the characteristic that concentration product values of oxalate and nickel hydroxide are similar; mixing the precursor material with a lithium source; sintering to synthesize the cathode material-lithium nickel manganese oxide. According to the method, the step of adopting only hydroxide as the precipitant under inert gas shielding is removed, so that the production cost is reduced; compared with lithium nickel manganese oxide prepared by taking only oxalate as the precipitant, the tap density is effectively improved; as the concentration product values of oxalate and nickel hydroxide are similar, the more uniform oxalate/nickel hydroxide compound precursor material can be obtained according to the control on the pH value of the solution.
Description
Technical field
The present invention relates to a kind of preparation method of lithium ion battery anode material nickel LiMn2O4.
Background technology
Along with social development, China's energy crisis and environmental pollution day by day serious, exploitation and the research of electrokinetic cell receive much concern.Lithium ion battery is a kind of high-energy battery that fast development is nearly ten years got up, and no matter from technical indicators such as life-span, specific energy and voltages, or from environment, it has become an important directions of China's New Energy Industry.Anode material nickel LiMn2O4 has that discharge voltage is high, Heat stability is good and the advantage such as price is lower, is considered to most potential positive electrode material.Use at present the precipitation reagent of the synthetic nickel lithium manganate material presoma of coprecipitation mostly to be oxalates, hydroxide, carbonate etc.Adopt oxalates or carbonate lower as the tap density of the synthetic nickel lithium manganate material of precipitation reagent, thereby the energy density in electrokinetic cell is less; And although employing hydroxide is higher as the synthetic nickel lithium manganate material tap density of precipitation reagent, need the protection of inert gas, also higher to the requirement of equipment.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of lithium ion battery anode material nickel LiMn2O4, i.e. two precipitation reagent coprecipitations.
For solving the problems of the technologies described above, the technical solution used in the present invention is: the preparation method of lithium ion battery anode material nickel LiMn2O4, comprises the following steps:
(1) take acetate, nitrate or the sulfate of nickel, manganese is transition metal source, according to mol ratio, is n (Ni): n (Mn)=1:1～3; Accurately weigh material, add appropriate distilled water to make the mixing salt solution A of nickel, manganese;
(2) usining sodium oxalate, potassium oxalate or ammonium oxalate as a kind of precipitation reagent, and using NaOH or potassium hydroxide as another kind of precipitation reagent, is n (C in molar ratio
2o
4 2-): n (OH
-)=0.5～2:1 configuration precipitant solution B;
(3) mixing salt solution A and precipitant solution B are added in the container that fills distilled water simultaneously, under the condition that low whipping speed is 200～800r/min, and by control, add the speed of precipitation reagent, regulating the pH value of reactant liquor is 8.5～10.5; In whole course of reaction, the temperature of reactant liquor is 25～80 ℃, reacts washing after 0.5～6 hour, dry, obtains the presoma of manganese oxalate/nickel hydroxide;
(4) presoma step (3) being obtained is placed in pre-burning 4～7h under the environment of 400～600 ℃, by the product after pre-burning, according to mol ratio, be that n (Li): n (Ni+Mn)=1.05～2.10:2 mixes with lithium nitrate, lithium carbonate, lithium hydroxide or lithium acetate, obtain mixture;
(5) mixture of step (4) is calcined to 6～18h at 750～1000 ℃, then, at 600～750 ℃ of annealing in process 4～14h, obtain lithium ion battery anode material nickel LiMn2O4.
The invention has the beneficial effects as follows:
(1) because the solubility product of manganese oxalate and nickel hydroxide is close, be respectively 1.1 * 10
-15mol/L and 2.0 * 10
-15mol/L; And the solubility product of manganous hydroxide and nickel oxalate is relatively large, be respectively 1.9 * 10
-13mol/L and 4.0 * 10
-10mol/L.By controlling the pH value of solution, prepare nickel hydroxide/manganese oxalate composite precursor, thereby saved, to adopt only hydroxide be the step that precipitation reagent needs inert gas shielding, reduced production cost;
(2) compare with the nickel LiMn2O4 that only uses oxalates to prepare for precipitation reagent, tap density is effectively improved; Because the solubility product of manganese oxalate and nickel hydroxide is close, thereby according to the control of pH, can obtain manganese oxalate/nickel hydroxide persursor material more uniformly.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is the synthetic spinel nickel LiMn2O4 of the embodiment of the present invention 1 and the charging and discharging curve that lithium metal forms simulated battery.
Fig. 2 is the charging and discharging curve that the embodiment of the present invention 2 synthetic spinel nickel LiMn2O4s and lithium metal form simulated battery.
Embodiment
Embodiment 1:
(1) n (Ni): n (Mn)=1:3 in molar ratio, accurately weighs manganese sulfate, nickelous sulfate, adds appropriate distilled water to be configured to mixed solution A.
(2) by the mol ratio of sodium oxalate and NaOH, be 1.5:1 configuration precipitant solution B.
(3) mixing salt solution A and precipitant solution B are added simultaneously in the container that contains distilled water, under the condition that low whipping speed is 300r/min, by controls, add pH value in the speed adjusting reactant liquor of precipitation reagent in 9.5 left and right.In whole course of reaction, the temperature of reactant liquor is 40 ℃, reacts washing after 3 hours, dry, obtains the presoma of manganese oxalate/nickel hydroxide.
(4) presoma step (3) being obtained is placed in pre-burning 6h under the environment of 500 ℃, by the product lithium carbonate after pre-burning, according to mol ratio, is that n (Li): n (Ni+Mn)=1.05:2 mixes, and obtains mixture.
(5) mixture step (4) being obtained, at 800 ℃ of calcining 7h, then at 700 ℃ of annealing in process 10h, obtains having the lithium ion battery anode material nickel LiMn2O4 of good spinel structure.
Embodiment 2:
(1) n (Ni): n (Mn)=1:3 in molar ratio, accurately weighs manganese sulfate, nickelous sulfate, adds appropriate distilled water to be configured to mixed solution A.
(2) by the mol ratio of potassium oxalate and NaOH, be 1.5:1 configuration precipitant solution B.
(3) mixing salt solution A and precipitant solution B are added simultaneously in the container that contains distilled water, under the condition that low whipping speed is 300r/min, by controls, add pH value in the speed adjusting reactant liquor of precipitation reagent in 9.3 left and right.In whole course of reaction, the temperature of reactant liquor, at 50 ℃, is reacted washing after 3 hours, dry, obtains the presoma of manganese oxalate/nickel hydroxide.
(4) presoma step (3) being obtained is placed in pre-burning 6h under the environment of 500 ℃, by the product after pre-burning, is that n (Li): n (Ni+Mn)=1.05:2 mixes with lithium carbonate according to mol ratio, obtains mixture.
(5) mixture step (4) being obtained is at 800 ℃ of calcining 7h, and then 700 ℃ of annealing in process 10h, obtains having the lithium ion battery anode material nickel LiMn2O4 of good spinel structure.
Embodiment 3:
(1) n (Ni): n (Mn)=1:3 in molar ratio, accurately weighs manganese sulfate, nickelous sulfate, adds appropriate distilled water to be configured to mixed solution A;
(2) be in molar ratio n (C
2o
4 2-): n (OH
-)=1.5:1 configures potassium oxalate, ammonium oxalate and potassium hydroxide precipitant solution B, wherein n (potassium oxalate): n (ammonium oxalate)=2:1;
(3) mixing salt solution A and precipitant solution B are added simultaneously in the container that contains distilled water, under the condition that low whipping speed is 300r/min, by controls, add pH value in the speed adjusting reactant liquor of precipitation reagent in 9.8 left and right.In addition, in whole course of reaction, the temperature of reactant liquor, at 50 ℃, is reacted washing after 3 hours, dry, obtains the presoma of manganese oxalate/nickel hydroxide;
(4) presoma step (3) being obtained is placed in pre-burning 6h under the environment of 600 ℃, by the product after pre-burning, is that n (Li): n (Ni+Mn)=1.05:2 mixes with lithium carbonate according to mol ratio, the mixture that obtains mixing;
(5) mixture step (4) being obtained, at 800 ℃ of calcining 7h, then at 700 ℃ of annealing in process 10h, obtains having the lithium ion battery anode material nickel LiMn2O4 of good spinel structure.
Embodiment 4:
(1) n (Ni): n (Mn)=1:1 in molar ratio, accurately weighs manganese sulfate, nickelous sulfate, adds appropriate distilled water to be configured to mixed solution A;
(2) be in molar ratio n (C
2o
4 2-): n (OH
-)=0.5:1 configuration potassium oxalate and potassium hydroxide precipitant solution B;
(3) mixing salt solution A and precipitant solution B are added simultaneously in the container that contains distilled water, under the condition that low whipping speed is 300r/min, by controls, add pH value in the speed adjusting reactant liquor of precipitation reagent in 9.3 left and right.In addition, in whole course of reaction, the temperature of reactant liquor, at 50 ℃, is reacted washing after 3 hours, dry, obtains the presoma of manganese oxalate/nickel hydroxide; .
(4) presoma step (3) being obtained is placed in pre-burning 7h under the environment of 500 ℃, by the product after pre-burning, is that n (Li): n (Ni+Mn)=1.05:1 mixes with lithium carbonate according to mol ratio, the mixture that obtains mixing;
(5) mixture step (4) being obtained, at 950 ℃ of calcining 10h, then at 700 ℃ of annealing in process 10h, obtains having the lithium ion battery anode material nickel LiMn2O4 of layer structure.
Embodiment 5:
The present embodiment and embodiment 3 differences are: the pH value in step (3) is controlled at 10.5 left and right, and the sintering temperature in step (5) is that the sintering time in 1000 ℃ and step (5) is 6h.
Embodiment 6:
The present embodiment and embodiment 2 differences are: the pH value in step (3) is controlled at 8.5 left and right, and the sintering temperature in step (5) is 750 ℃.Sintering time in step (5) is 18h, and the annealing conditions in step (5) is 600 ℃ of calcining 4h.
The nickel lithium manganate material of gained in above-described embodiment 1 and embodiment 2 is assembled into respectively to button cell, in battery, positive electrode ratio is nickel LiMn2O4: conductive agent: binding agent=80:10:10, adopt Clgard2300 type barrier film, to electrode, it is metal lithium sheet, with 0.2C, carry out charge-discharge performance test, charging/discharging voltage scope is 3.0-4.3V.As shown in Figure 1, the charging and discharging curve of the sample that embodiment 2 obtains after after tested as shown in Figure 2 for the charging and discharging curve of the sample that embodiment 1 obtains after after tested.From charging and discharging curve, can find out, in 4.7V left and right, present charge and discharge platform, illustrate that synthetic material is spinelle nickel lithium manganate material.
Above-described embodiment of the present invention, does not form limiting the scope of the present invention.Any modification of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in claim protection range of the present invention.
Claims (1)
1. the preparation method of lithium ion battery anode material nickel LiMn2O4, is characterized in that comprising the following steps:
(1) take acetate, nitrate or the sulfate of nickel, manganese is transition metal source, according to mol ratio, is n (Ni): n (Mn)=1:1～3; Accurately weigh material, add appropriate distilled water to make the mixing salt solution A of nickel, manganese;
(2) usining sodium oxalate, potassium oxalate or ammonium oxalate as a kind of precipitation reagent, and using NaOH or potassium hydroxide as another kind of precipitation reagent, is n (C in molar ratio
2o
4 2-): n (OH
-)=0.5～2:1 configuration precipitant solution B;
(3) mixing salt solution A and precipitant solution B are added in the container that fills distilled water simultaneously, under the condition that low whipping speed is 200～800r/min, and by control, add the speed of precipitation reagent, regulating the pH value of reactant liquor is 8.5～10.5; In whole course of reaction, the temperature of reactant liquor is 25～80 ℃, reacts washing after 0.5～6 hour, dry, obtains the presoma of manganese oxalate/nickel hydroxide;
(4) presoma step (3) being obtained is placed in pre-burning 4～7h under the environment of 400～600 ℃, by the product after pre-burning, according to mol ratio, be that n (Li): n (Ni+Mn)=1.05～2.10:2 mixes with lithium nitrate, lithium carbonate, lithium hydroxide or lithium acetate, obtain mixture;
(5) mixture of step (4) is calcined to 6～18h at 750～1000 ℃, then, at 600～750 ℃ of annealing in process 4～14h, obtain lithium ion battery anode material nickel LiMn2O4.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106684350A (en) * | 2016-12-21 | 2017-05-17 | 桑顿新能源科技有限公司 | Preparation method of lithium nickel manganese oxide serving as high-voltage positive electrode material |
| CN108288711A (en) * | 2018-02-12 | 2018-07-17 | 成都理工大学 | A kind of quaternary lithium-ion battery positive electrode material and preparation method |
| CN109811412A (en) * | 2018-12-28 | 2019-05-28 | 广东邦普循环科技有限公司 | A kind of stratiform nickel lithium manganate cathode material of monocrystalline pattern and preparation method thereof |
| CN110137445A (en) * | 2019-03-26 | 2019-08-16 | 广西卓能新能源科技有限公司 | Battery anode slice, lithium ion battery, stratiform nickel ion doped and preparation method thereof |
| CN114408987A (en) * | 2022-03-30 | 2022-04-29 | 宜宾锂宝新材料有限公司 | Nickel-cobalt-manganese precursor, ternary cathode material and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106684350A (en) * | 2016-12-21 | 2017-05-17 | 桑顿新能源科技有限公司 | Preparation method of lithium nickel manganese oxide serving as high-voltage positive electrode material |
| CN108288711A (en) * | 2018-02-12 | 2018-07-17 | 成都理工大学 | A kind of quaternary lithium-ion battery positive electrode material and preparation method |
| CN109811412A (en) * | 2018-12-28 | 2019-05-28 | 广东邦普循环科技有限公司 | A kind of stratiform nickel lithium manganate cathode material of monocrystalline pattern and preparation method thereof |
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| CN110137445A (en) * | 2019-03-26 | 2019-08-16 | 广西卓能新能源科技有限公司 | Battery anode slice, lithium ion battery, stratiform nickel ion doped and preparation method thereof |
| CN114408987A (en) * | 2022-03-30 | 2022-04-29 | 宜宾锂宝新材料有限公司 | Nickel-cobalt-manganese precursor, ternary cathode material and preparation method thereof |
| CN114408987B (en) * | 2022-03-30 | 2022-06-21 | 宜宾锂宝新材料有限公司 | Nickel-cobalt-manganese precursor, ternary cathode material and preparation method thereof |
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Application publication date: 20140212 Assignee: NANJING GUOXUAN BATTERY CO., LTD. Assignor: Hefei Guoxuan High-Tech Power Energy Co., Ltd. Contract record no.: 2017320000046 Denomination of invention: Method for preparing nickel lithium manganate serving as cathode material of lithium ion battery Granted publication date: 20160330 License type: Exclusive License Record date: 20170306 |