CN103746108A - Preparation method of lithium ion battery positive electrode material doped with hollow nickel lithium manganate structure - Google Patents
Preparation method of lithium ion battery positive electrode material doped with hollow nickel lithium manganate structure Download PDFInfo
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- 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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- 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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Abstract
The invention provides a preparation method of a lithium ion battery positive electrode material doped with a hollow nickel lithium manganate structure. The method comprises the following steps: 1, preparing a carbon sphere; 2, preparing hollow nickel lithium manganate doped with magnesium; and 3, preparing nickel lithium manganate cladding of a magnesium-doped hollow structure. According to the invention, the cycle life of a battery can be prolonged greatly, and the cycle efficiency can be kept about at 90%.
Description
Technical field
The present invention relates to the preparation method in a kind of cell positive material, relate in particular to a kind of preparation, the doping of nickel LiMn2O4 and surface coated method of hollow ball structure nickel lithium manganate material.
Background technology
Nickel LiMn2O4 surface is directly to contact with electrolyte, Mn in nickel lithium manganate material
3+soluble in electrolyte is molten, poor electric conductivity, the utilance of material are low, lithium ion diffusion is slow, cause thus the reversibility of battery poor, in cyclic process under capability retention low and high temperature or the problem such as the cycle performance under large multiplying power is poor.One of common solution, doping and Li in nickel lithium manganate material
+, Ni
2+, Mn
4+, O
2-other ions that plasma effect power is stronger occupy relevant position, the formation chemical bond more stable than Mn-O bond energy of being combined with O stablized nickel LiMn2O4 lattice structure, effectively suppress because Mn3+ is dissolved in the problem that electrolyte subsides nickel LiMn2O4 lattice, thereby can improve capability retention in the reversibility of battery and cyclic process; Two of its solution, the protective material that coated one deck directly contacts with electrolyte on the surface of nickel lithium manganate material, the oxidation of the metal ion that can have a high valence state of inhibition to electrolyte, makes electrolyte more stable, can also in certain degree, stop Mn
3+stripping, when playing protective material stability action, can also improve under the conductivity, high temperature of material or stability and capability retention in the cyclic process under large multiplying power.For the utilance of nickel LiMn2O4, low and lithium ion spreads slow problem, and nickel LiMn2O4 is prepared into hollow-core construction, can greatly reduce like this distance that lithium ion shuttles back and forth, and improves the utilance of material.
But in current technology, the nickel LiMn2O4 size of hollow-core construction differs; Nickel LiMn2O4 to hollow-core construction adulterates, and can not guarantee the particular location of doping; The nickel LiMn2O4 of hollow-core construction is carried out to surface and be coated, the area size that coating layer is coated and the thickness evenness of coating layer differ.
Summary of the invention
In order to solve above technical problem.The present invention is applied to the method for multiple performance change in nickel lithium manganate material simultaneously, has broken through the mode of thinking that in the past only changes a kind of performance by single mode, makes the performance of material have more advantage, and concrete operation step is as follows:
Steps A: the preparation of carbon ball: glucose is dissolved in deionized water, high-speed stirred to solution presents clarification shape, again solution is transferred in reactor, react 10 to 14 hours at 160 ℃ to 200 ℃ again, naturally cool to again room temperature, product in reactor is used respectively to deionized water, absolute ethyl alcohol centrifuge washing, remove dextrose components remaining in product, then after vacuumize, obtain the carbon ball of black.
Step B: nickel acetate and manganese acetate are dissolved in absolute ethyl alcohol, again concentrated hydrochloric acid is slowly added drop-wise to magnetic agitation in solution, in this system, add 1-1.5mol/L carbon ball again, with ultrasonic echography until form the state of homogeneous, again product is transferred to 160 ℃ to 200 ℃ constant temperature 6-10 hour in reactor, after complete reaction, naturally cool to the sediment that room temperature obtains black, again black precipitate is used respectively to deionized water, absolute ethyl alcohol centrifuge washing, remove not impurity, after vacuumize, obtain the presoma of carbon/nickel oxide, presoma is transferred in Muffle furnace, under 500-700 ℃ of constant temperature, calcine 3-5 hour, obtain the Ni, Mn oxide of hollow-core construction.
Step C: lithium acetate, magnesium acetate are all dissolved in absolute ethyl alcohol, according to the ratio of amount of substance in chemical molecular formula, the ratio that is lithium acetate and magnesium acetate amount of substance is 1.1:2, wherein lithium acetate consumption have 10% excessive, be used for making up the loss in sintering process, the Ni, Mn oxide of hollow-core construction is added in the solution of lithium acetate, with ultrasonic echography until form the state of homogeneous, continue ultrasonic absolute ethyl alcohol to be evaporated, then be transferred to and in Muffle furnace, carry out solid phase reaction, calcining at constant temperature, obtains the nickel LiMn2O4 doped with the hollow-core construction of magnesium;
Step D: the coated preparation of nickel LiMn2O4 of magnesium-doped hollow-core construction: slowly drip ammoniacal liquor under the state that liquor argenti nitratis ophthalmicus is stirred, until the precipitation generating is just completely dissolved and is presented transparence, be heated to 65-85 ℃ and carry out water-bath, the nickel LiMn2O4 powder of mixing magnesium hollow-core construction that described step C is prepared is dissolved in and in absolute ethyl alcohol, adds thermal agitation, with ultrasonic cleaner, solution is disperseed simultaneously, add 5mL formaldehyde, liquor argenti nitratis ophthalmicus is slowly joined in this solution, stirring is fully reacted it, to product deionized water centrifuge washing, after vacuumize, obtain the coated nickel LiMn2O4 composite material of mixing magnesium hollow-core construction of silver.
Wherein, the amount that formaldehyde and liquor argenti nitratis ophthalmicus add makes it that silver mirror reaction fully occur.
Preferably, in described steps A and B, in vacuum drying chamber, under 60 ℃ of constant temperature, be dried 6 hours.
Preferably, the temperature of calcining under constant temperature is 800 ℃, and the time is 6 hours.
Preferably, in described step D, the concentration of liquor argenti nitratis ophthalmicus is 0.2mol/L.
Preferably, in described step D, add the time of formaldehyde for disperseing latter 5 to 15 minutes.
Preferably, in described step D, the temperature of vacuum drying chamber is 100 ℃.
Preferably, carbon ball with the ratio of the amount of substance of nickel acetate is: 1-1.5.
Preferably, the ratio of lithium acetate and manganese acetate amount of substance is 1.1:2, wherein lithium acetate consumption have 10% excessive, be used for making up the loss in sintering process.
In this invention, consider the situation that the size of hollow-core construction nickel LiMn2O4 differs, carbon ball is screened, within the size of its carbon ball is controlled to inhomogeneity scope, control the uniformity of hollow-core construction nickel lithium manganate material size, and greatly improved the efficiency of lithium ion in deintercalation and inserting process, the utilance of material is improved, the actual specific capacity (140mAh/g) of material almost approaches theoretical numerical value (146.7 mAh/g); Actual magnesium-doped position can not be clear and definite, but can know magnesium approximate location in nickel LiMn2O4 structure by calculating emulation; For the thickness problem of coated areal extent, coating layer, the mode that time, temperature, the high-speed stirred of reacting by prolongation reacted solves, coating layer has suppressed under the condition of high temperature effectively, the resolution problem of battery electrolyte, make the cycle life of battery obtain promoting greatly, and cycle efficieny remain on 90% left and right.
Accompanying drawing explanation
Fig. 1 is the hollow-core construction nickel LiMn2O4 schematic diagram that the present invention prepares.
Fig. 2 is the SEM figure of the hollow-core construction nickel LiMn2O4 in an embodiment of the present invention.
Fig. 3 be the present invention adulterate and coated after nickel LiMn2O4 structural representation.
Fig. 4 be hollow-core construction nickel LiMn2O4 of the present invention adulterate and be coated after SEM figure.
Fig. 5 be hollow-core construction nickel LiMn2O4 of the present invention adulterate and be coated after charge and discharge cycles curve.
Fig. 6 be hollow-core construction nickel LiMn2O4 of the present invention adulterate and be coated after 100 charge and discharge cycles curves.
Embodiment
Below in conjunction with accompanying drawing, preferably embodiment of the present invention is described in further detail:
Embodiment 1:
1, the preparation of carbon ball
The glucose of 9g is dissolved in deionized water, and high-speed stirred half an hour is until solution presents clarification shape, then solution is transferred in the reactor of 100mL to isothermal reaction 12 hours under the environment of 180 ℃.When by the time naturally cooling to room temperature, the product in reactor is used respectively to deionized water, absolute ethyl alcohol centrifuge washing three times, remove dextrose components remaining in product.In vacuum drying chamber, under 60 ℃ of constant temperature, be dried 6 hours, will obtain the carbon ball of black.
2, mix the preparation of magnesium Hollow Nickel LiMn2O4
1. the manganese acetate of the nickel acetate of 0.5mol, 1.5mol is dissolved in the absolute ethyl alcohol of 40mL, then concentrated hydrochloric acid is slowly added drop-wise in solution to magnetic agitation 10 minutes, then to the carbon ball that adds 1mol in this system, with ultrasonic echography until form the state of homogeneous.The product of above-mentioned system is transferred in the reactor of 100mL to 180 ° of constant temperature 8 hours.After complete reaction, when naturally cooling to room temperature, obtain the sediment of black.Black precipitate is used respectively to deionized water, absolute ethyl alcohol centrifuge washing three times, remove the impurity of failing to participate in reaction.In vacuum drying chamber, under 60 ℃ of constant temperature, be dried 6 hours, obtain the presoma of carbon/nickel oxide.Presoma is transferred in Muffle furnace, under 600 ℃ of constant temperature, calcined 4 hours, obtain the Ni, Mn oxide of hollow-core construction.
2. lithium acetate, magnesium acetate are all dissolved in absolute ethyl alcohol, according to the ratio of 1.1:2 amount of substance, the Ni, Mn oxide of hollow-core construction is added in the solution of lithium acetate, with ultrasonic echography until form the state of homogeneous, continue ultrasonic absolute ethyl alcohol to be evaporated, then be transferred to and in Muffle furnace, carry out solid phase reaction, under 800 ℃ of constant temperature, calcine 6 hours, finally obtain the nickel LiMn2O4 doped with the hollow-core construction of magnesium.
3, the coated preparation of nickel LiMn2O4 of magnesium-doped hollow-core construction
The liquor argenti nitratis ophthalmicus of configuration 0.2mol/L, slowly drips ammoniacal liquor on magnetic stirring apparatus under the state stirring, until the precipitation generating is just completely dissolved and presented transparence, be heated to 75 ℃ and carry out water-bath.The nickel LiMn2O4 powder of mixing magnesium hollow-core construction that top is prepared is dissolved in absolute ethyl alcohol and adds thermal agitation, with ultrasonic cleaner, solution is disperseed simultaneously, disperses to add after 10 minutes the formaldehyde of 5mL.Liquor argenti nitratis ophthalmicus is slowly joined in this solution, and magnetic agitation 30 minutes, fully reacts it.To product deionized water centrifuge washing three times, dry under 100 ℃ of constant temperature in vacuum drying chamber, finally obtain the coated nickel LiMn2O4 composite material of mixing magnesium hollow-core construction of silver.
Embodiment 2
1, the preparation of carbon ball
The glucose of 13.5g is dissolved in a certain amount of deionized water, and high-speed stirred half an hour is until solution presents clarification shape, then solution is transferred in the reactor of 100mL to isothermal reaction 10 hours under the environment of 2000 ℃.When by the time naturally cooling to room temperature, the product in reactor is used respectively to deionized water, absolute ethyl alcohol centrifuge washing three times, remove dextrose components remaining in product.In vacuum drying chamber, under 60 ℃ of constant temperature, be dried 6 hours, will obtain the carbon ball of black.
2, mix the preparation of magnesium Hollow Nickel LiMn2O4
1. the manganese acetate of the nickel acetate of 0.75mol, 7.5mol is dissolved in the absolute ethyl alcohol of 40mL, then concentrated hydrochloric acid is slowly added drop-wise in solution to magnetic agitation 10 minutes, then add 1.5mol carbon ball in this system, with ultrasonic echography until form the state of homogeneous.The product of above-mentioned system is transferred in the reactor of 100mL to 200 ℃ of constant temperature 6 hours.After complete reaction, when naturally cooling to room temperature, obtain the sediment of black.Black precipitate is used respectively to deionized water, absolute ethyl alcohol centrifuge washing three times, remove the impurity of failing to participate in reaction.In vacuum drying chamber, under 60 ℃ of constant temperature, be dried 6 hours, obtain the presoma of carbon/nickel oxide.Presoma is transferred in Muffle furnace, under 600 ℃ of constant temperature, calcined 4 hours, obtain the Ni, Mn oxide of hollow-core construction;
2. lithium acetate, magnesium acetate are all dissolved in absolute ethyl alcohol, according to the ratio of 1.1:2 amount of substance, the Ni, Mn oxide of hollow-core construction is added in the solution of lithium acetate, with ultrasonic echography until form the state of homogeneous, continue ultrasonic absolute ethyl alcohol to be evaporated, then be transferred to and in Muffle furnace, carry out solid phase reaction, under 800 ℃ of constant temperature, calcine 6 hours, finally obtain the nickel LiMn2O4 doped with the hollow-core construction of magnesium.
3, the coated preparation of nickel LiMn2O4 of magnesium-doped hollow-core construction
The liquor argenti nitratis ophthalmicus of configuration 0.2mol/L, slowly drips ammoniacal liquor on magnetic stirring apparatus under the state stirring, until the precipitation generating is just completely dissolved and presented transparence, be heated to 80 ℃ and carry out water-bath.The nickel LiMn2O4 powder of mixing magnesium hollow-core construction that top is prepared is dissolved in absolute ethyl alcohol and adds thermal agitation, with ultrasonic cleaner, solution is disperseed simultaneously, disperses to add after 10 minutes the formaldehyde of 5mL.Liquor argenti nitratis ophthalmicus is slowly joined in this solution, and magnetic agitation 30 minutes, fully reacts it.To product deionized water centrifuge washing three times, dry under 100 ℃ of constant temperature in vacuum drying chamber, finally obtain the coated nickel LiMn2O4 composite material of mixing magnesium hollow-core construction of silver.
The innovation of this programme and other schemes is as follows:
1, the nickel LiMn2O4 of preparation is different from traditional entity structure, and what in this programme, prepare is hollow-core construction, and the granular size homogeneous preparing, and covered effect is good, and its schematic diagram and SEM master drawing are as illustrated in fig. 1 and 2.
2, the nickel lithium manganate material preparing has embodied very large advantage in capacity and cycle life and efficiency thereof, as shown in Fig. 3 to 6, the specific capacity of actual test is at 140mAh/g, this and theoretic 146.7 mAh/g very approach, and the platform occurring at 4.1V place obviously reduces, and the charge and discharge platform occurring in 4.75V left and right is very wide.Especially in charge and discharge cycles process, cycle efficieny remains on 90% left and right, and consumption rate is lower, and the utilance of material is higher.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Claims (8)
1. a preparation method for Hollow Nickel LiMn2O4 structure doped lithium ion battery cathode material, is characterized in that, comprises following step:
Steps A: the preparation of carbon ball: glucose is dissolved in deionized water, high-speed stirred to solution presents clarification shape, again solution is transferred in reactor, react 10 to 14 hours at 160 ℃ to 200 ℃ again, naturally cool to again room temperature, product in reactor is used respectively to deionized water, absolute ethyl alcohol centrifuge washing, remove glucose remaining in product, then after vacuumize, obtain the carbon ball of black;
Step B: nickel acetate and manganese acetate are dissolved in absolute ethyl alcohol, again concentrated hydrochloric acid is slowly added drop-wise to magnetic agitation in solution, in this system, add carbon ball again, with ultrasonic echography until form the state of homogeneous, again product is transferred to 160 ℃ to 200 ℃ constant temperature 6-10 hour in reactor, after complete reaction, naturally cool to the sediment that room temperature obtains black, again black precipitate is used respectively to deionized water, absolute ethyl alcohol centrifuge washing, remove impurity, after vacuumize, obtain the presoma of carbon/nickel oxide, presoma is transferred in Muffle furnace, under 500-700 ℃ of constant temperature, calcine 3-5 hour, obtain the Ni, Mn oxide of hollow-core construction,
Step C: lithium acetate, magnesium acetate are all dissolved in absolute ethyl alcohol, again the Ni, Mn oxide of hollow-core construction is added in the solution of lithium acetate, with ultrasonic echography until form the state of homogeneous, continue ultrasonic absolute ethyl alcohol to be evaporated, then be transferred to and in Muffle furnace, carry out solid phase reaction, calcining at constant temperature, obtains the nickel LiMn2O4 doped with the hollow-core construction of magnesium;
Step D: the coated preparation of nickel LiMn2O4 of doped hollow structure: slowly drip ammoniacal liquor under the state that liquor argenti nitratis ophthalmicus is stirred, until the precipitation generating is just completely dissolved and is presented transparence, be heated to 65-85 ℃ and carry out water-bath, the nickel LiMn2O4 powder of mixing magnesium hollow-core construction that described step C is prepared is dissolved in and in absolute ethyl alcohol, adds thermal agitation, with ultrasonic cleaner, solution is disperseed simultaneously, add formaldehyde, liquor argenti nitratis ophthalmicus is slowly joined in this solution, stirring is fully reacted it, to product deionized water centrifuge washing, after vacuumize, obtain the coated nickel LiMn2O4 composite material of mixing magnesium hollow-core construction of silver.
2. the preparation method of Hollow Nickel LiMn2O4 structure doped lithium ion battery cathode material as claimed in claim 1, is characterized in that, in described steps A and B, in vacuum drying chamber, under 60 ℃ of constant temperature, is dried 6 hours.
3. the preparation method of Hollow Nickel LiMn2O4 structure doped lithium ion battery cathode material as claimed in claim 1, is characterized in that, the temperature of calcining under constant temperature is 800 ℃, and the time is 6 hours.
4. the preparation method of Hollow Nickel LiMn2O4 structure doped lithium ion battery cathode material as claimed in claim 1, is characterized in that, in described step D, the concentration of liquor argenti nitratis ophthalmicus is 0.2mol/L.
5. the preparation method of Hollow Nickel LiMn2O4 structure doped lithium ion battery cathode material as claimed in claim 1, is characterized in that, in described step D, adds the time of formaldehyde for disperseing latter 5 to 15 minutes.
6. the preparation method of Hollow Nickel LiMn2O4 structure doped lithium ion battery cathode material as claimed in claim 1, is characterized in that, in described step D, the temperature of vacuum drying chamber is 100 ℃.
7. the preparation method of Hollow Nickel LiMn2O4 structure doped lithium ion battery cathode material as claimed in claim 1, is characterized in that, in described step B, carbon ball with the ratio of the amount of substance of nickel acetate is: 1-1.5.
8. the preparation method of Hollow Nickel LiMn2O4 structure doped lithium ion battery cathode material as claimed in claim 1, is characterized in that, in described step B, the ratio of lithium acetate and manganese acetate amount of substance is 1.1:2.
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| CN108172814A (en) * | 2018-02-02 | 2018-06-15 | 云南民族大学 | A kind of silver simple substance coating spinelle type LiMn2O4Composite material and preparation method thereof |
| CN110165199A (en) * | 2019-07-04 | 2019-08-23 | 银隆新能源股份有限公司 | A kind of positive electrode of modification and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106025260A (en) * | 2016-07-06 | 2016-10-12 | 上海交通大学 | Ternary cathode material of hollow spherical nano-structure and preparing method thereof |
| CN107394126A (en) * | 2017-06-09 | 2017-11-24 | 安徽零度新能源科技有限公司 | A kind of positive composite material of lithium battery with the high life |
| CN108172814A (en) * | 2018-02-02 | 2018-06-15 | 云南民族大学 | A kind of silver simple substance coating spinelle type LiMn2O4Composite material and preparation method thereof |
| CN110165199A (en) * | 2019-07-04 | 2019-08-23 | 银隆新能源股份有限公司 | A kind of positive electrode of modification and preparation method thereof |
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| CN114497529A (en) * | 2021-12-30 | 2022-05-13 | 贵州梅岭电源有限公司 | Preparation method of silver nanoparticle coated lithium manganate positive electrode material |
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