CN102800856A - Preparation method of manganic acid-nickel-lithium positive electrode with high specific energy and high power - Google Patents

Preparation method of manganic acid-nickel-lithium positive electrode with high specific energy and high power Download PDF

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CN102800856A
CN102800856A CN201210316086XA CN201210316086A CN102800856A CN 102800856 A CN102800856 A CN 102800856A CN 201210316086X A CN201210316086X A CN 201210316086XA CN 201210316086 A CN201210316086 A CN 201210316086A CN 102800856 A CN102800856 A CN 102800856A
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nickel
labeled
solution
lithium
acetate
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郑圣泉
陈红梅
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ZHUZHOU TITAN POWER TECH CO LTD
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ZHUZHOU TITAN POWER TECH CO LTD
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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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a preparation method of a manganic acid-nickel-lithium positive electrode with high specific energy and high power. According to the preparation, a sol-gel method is adopted to the material; a precursor of the raw materials prepared with one of the nickel, manganese, lithium acetate salt and oxalic acid, ammonium oxalate, citric acid and ammonium citrate serving as a chelating agent is adopted to decompose acetate in the air at 400 to 450 DEG C, then slightly grinded and roasted for 1 to 2 hours under an oxygen condition at 850 to 900 DEG C, and finally annealed to roast for 6 to 10 hours at 500 to 600 DEG C so as to obtain a product of LiNi0.5Mn1.504 which has tap density up to 2.0 to 2.5 and has regular shape and appearance. A simulated battery prepared by positive electrode materials can be charged and discharged under constant current of rate of 1C within the range of 0.8 to 4.9V, and the capacity in the first discharging is more than 132mAh/g, and the capacity is up to 134mAh/g after cycling at 218 times, as the results shown, the material has high specific capacity and long cycle life.

Description

A kind of high specific energy high power mangaic acid nickel lithium anode preparation method
Technical field
The present invention relates to a kind of high specific energy high power mangaic acid nickel lithium anode preparation method, belong to energy and material, new material and lithium ion battery preparing technical field.
Background technology
In recent years, along with the requirement of the serious day by day and electronic product lightness of energy environment problem, people deepen continuously to the research of lithium rechargeable battery.Business-like anode material for lithium-ion batteries LiCoO 2Because price is high, and is toxic, people make great efforts seeking its substitute always.LiMn2O4 receives much attention owing to cheap, nontoxic.And the LiNi of adding nickel 0.5Mn 1.5O 4Charge and discharge platform is the 5V material between 4.6 ~ 4.8V, and theoretical capacity can reach 147mAh/g, has higher energy density, is hopeful to be applied as electrokinetic cell.
Summary of the invention
Patent of the present invention to the effect that adopts a kind of LiNi that does the chelating agent preparation in nickel manganese lithium acetate and oxalic acid, ammonium oxalate, citric acid, the Triammonium citrate 0.5Mn 1.5O 4The product tap density reach 2.0 ~ 2.5 and pattern regular.The synthetic material of the sol-gel method that adopts has better electrochemical performance.
Presoma makes acetate decompose in 400 ~ 450 ℃ of air during with Prepared by Sol Gel Method, after slight the grinding, in 850 ℃ ~ 900 ℃ oxygen atmospheres, calcines and is annealed to 500 ~ 600 ℃ of calcining 6 ~ 10h after 1 ~ 2h and obtains specimen material.
Through physical characteristics such as XRD, SEM, BET exosyndrome material structure and morphologies, material electrochemical stability is tested through means such as constant current charge-discharge, cyclic voltammetric, AC impedances.More different synthesis conditions, different PH, and chemical property detects under the same sample different condition.
The object of the present invention is to provide a kind of function admirable, cheap high specific energy high power mangaic acid nickel lithium anode preparation method, this method is simple, can prepare the chemical property that the regular tap density of pattern is high, optimized material.
The technical scheme of this method is following:
A kind of high specific energy high power mangaic acid nickel lithium anode preparation method is characterized in that this method carries out according to the following steps:
1) takes by weighing manganese source manganese salt, nickel source nickel salt, lithium source lithium salts respectively by stoichiometric proportion, be mixed with the manganese nickel lithium mixed solution of (Ni+Mn+Li) 0.1525Mol with deionized water dissolving;
2) take by weighing chelating agent: a kind of concentration that is mixed with of oxalic acid, ammonium oxalate, citric acid, Triammonium citrate is 0.15mol solution;
3) ammonia spirit of preparation 25%;
4) with the solution ultrasonic dissolution or the heating for dissolving of step 1), again with step 2) solution under 60 ℃ of states, be stirred to dissolving;
5) with step 2) solution under 60 ℃ of states, be stirred to dissolving; Be warming up to 90 ℃ and continue the step 1) mixed solution that stirring will dissolve down, drop in consoluet step 2 solution; The dropping time is controlled at 30 ~ 60min;
6) then to 1) and 2) the ammoniacal liquor of mixed solution and dripping 25% to PH=6.5～7, be warming up to 98 ℃, be stirred to evaporate to dryness with 3HZ, be grass green;
7) with the grass green lump of step 6), in 90 ℃ of vacuumize 12-48h;
8) move into and to place Muffle furnace 400-450 ℃ of air sintering 4-6 hour in the crucible, 5～10 ℃ of programming rate per minutes are cooled to room temperature naturally;
9) the step 8) products therefrom is ground after, in air in 850～900 ℃ of calcining 1～2h after annealings down: 600～650 ℃, promptly obtain the product LiNi of high voltage, high-tap density, high power capacity excellent performance behind time 8～10h 0.5Mn 1.5O 4
The high specific energy high power mangaic acid nickel lithium anode material LiNi of the present invention's preparation 0.5Mn 1.5O 4, have higher tap density, can reach 2.0 ~ 2.5g/cm 3; And the product particle pattern is regular, extremely is helped particle surface coat and modify, and for further improving the product chemical property advantageous conditions is provided.Product has better electrochemical performance; Has very big using value in high specific energy, high power lithium ion cell field.
Description of drawings
Fig. 1 is the multiplying power with 1C of embodiment 1 said target product, voltage range be under 3.8 V～4.9 V first with 200 charge-discharge performances;
Fig. 2 is the SEM collection of illustrative plates of embodiment 1 said target product;
Fig. 3 is the XRD figure spectrum of embodiment 1 said target product;
Fig. 4 is the multiplying power with 1C of embodiment 2 said target products, voltage range be under 3.8 V～4.9 V first with 200 times enclosed pasture efficient and discharge capacity;
Fig. 5 is embodiment 2 said target products; With the multiplying power of 0.5C, be the first charge-discharge performance under 3.6V～4.9 V in voltage range;
Fig. 6 to be embodiment 2 said target products be multiplying power with 0.5C is that under 3.5 V～4.9 V 1000 times discharge and recharge and cycle performance in voltage range;
The XRD figure spectrum that Fig. 7 for embodiment 2 said target products is.
Embodiment
Employed material, reagent all can obtain from general commercial sources among the following embodiment; Employed implementation method is conventional method.Embodiment further specifies the present invention, but does not limit the scope of the invention.
Embodiment 1:
The raw material that this enforcement is used: nickel acetate, manganese acetate, lithium acetate, Triammonium citrate, 25% ammoniacal liquor and deionized water.
(1) calculates the synthetic 0.05 mol target product of consumption of primary raw material according to the chemical formula of target product, take by weighing nickel acetate 6.3485 g, manganese acetate 18.5764 g, lithium acetate 5.40962 g and Triammonium citrate 37.0386 g according to stoichiometric proportion;
(2) get appropriate amount of deionized water and dissolve Ni salt, Mn salt, Li salt respectively, being configured to total concentration is the salting liquid A of 0.1525mol/L; The Triammonium citrate solution concentration is the salting liquid B of 0.15mol/L;
(3) B solution is placed blender, be warming up to 90 ℃, stir, under stirring, A solution is added in the blender with after B solution mixes fully, using 25% ammoniacal liquor adjust pH is to stop to drip in 6.5 ~ 7 o'clock, continues to be stirred to complete evaporate to dryness;
(4) with the gluey presoma of the light green color that obtains, under 90 ℃, carry out vacuumize, obtain anhydrous presoma;
(5) anhydrous presoma is transferred in the Muffle furnace 400～450 ℃ of preliminary treatment 4～6h in air, is cooled to room temperature naturally, porphyrize;
(6) again with pretreated presoma C in air atmosphere, 850～900 times calcining 1～2h after annealings: 600～650 ℃, time 8～10h naturally cools to room temperature afterwards and obtains black powder target product D.Programming rate 10 degree per minutes, cooling rate is 5 degree per minutes, promptly obtains the product LiNi of high voltage, high-tap density, high power capacity excellent performance afterwards 0.5Mn 1.5O 4
(7) the pole piece batching (is called for short PVDF according to the ratio of 8:1:1 with active material, acetylene black and binding agent polyvinylidene fluoride; Be dissolved in the 1-Methyl-2-Pyrrolidone) place ball mill mixing stirring ball-milling 3h to apply afterwards, blade thickness is with 150 or 200 microns; The slurry that obtains is coated on the aluminium foil, obtains the grey pole piece, the pole piece after applying is placed 70～80 ℃ the dry 4h of air dry oven, dry compressing tablet, section, weighing pole piece afterwards.Dry by the fire 2-24h.Se down for 120 ℃ at vacuum condition.Subsequently it is transferred to the glove box (water and oxygen content are less than 1 μ molL-1) of argon atmosphere protection; With it is positive pole; Adopt standard C elgard 2700 barrier films between both positive and negative polarity, assembling at last becomes the CR2025 button cell, and electrolyte is 1M LiPF6 EC:DMC=1:1 (v:v);
Fig. 1 is 3.8 V～4.9 V for the high specific energy high power of the lithium ion battery mangaic acid nickel lithium anode material for preparing according to above-mentioned embodiment in the scope of discharging and recharging, the constant current charge-discharge multiplying power be under 1 C first with 200 charging and discharging curves.As can be seen from the figure, along with the continuation of circulation, the specific capacity of material is not decay basically; Circulate first that specific capacity is 132 mAh/g, along with the continuation capacity of circulation rises, 200 specific capacities are 134.5 mAh/g, and capability retention reaches 100% with enclosed pasture efficient.Show that the high specific energy high power mangaic acid nickel lithium anode material that obtains that is synthesized has good cycle life and very high specific capacity, is applicable to suitability for industrialized production;
The high specific energy high power mangaic acid nickel lithium anode material SEM collection of illustrative plates of Fig. 2 for preparing according to above-mentioned embodiment;
The high specific energy high power mangaic acid nickel lithium anode material XRD figure spectrum of Fig. 3 for preparing according to above-mentioned embodiment.
Be the high specific energy high power of the lithium ion battery mangaic acid nickel lithium anode material embodiment 2 for preparing according to above-mentioned embodiment:
The raw material that this enforcement is used: nickel acetate, manganese acetate, lithium acetate, ammonium oxalate, 25% ammoniacal liquor and deionized water.
(1) calculates the synthetic 0.05 mol target product of consumption of primary raw material according to the chemical formula of target product, take by weighing nickel acetate 6.3485 g, manganese acetate 18.5764 g, lithium acetate 5.40962 g and ammonium oxalate 21.4236 g according to stoichiometric proportion;
(2) get appropriate amount of deionized water and dissolve Ni salt, Mn salt, Li salt respectively, being configured to total concentration is the salting liquid A1 of 0.1525mol/L; Ammonium oxalate solution concentration is the salting liquid B1 of 0.15mol/L;
(3) B1 solution is placed blender, be warming up to 90 ℃, stir.Under stirring, A1 solution is added in the blender with after B1 solution mixes fully, stop dropping when using 25% ammoniacal liquor adjust pH, continue to be stirred to complete evaporate to dryness as 7.0-7.5;
(4) with the light green color lump shape presoma that obtains, under 90 ℃, carry out vacuumize, obtain anhydrous presoma;
(5) anhydrous presoma is transferred in the Muffle furnace 400～450 ℃ of preliminary treatment 4～6h in air, is cooled to room temperature naturally, porphyrize;
(6) again with pretreated presoma C1 in air atmosphere; 850～900 times calcining 1～2h after annealings: 600～650 ℃; Time 8～10h naturally cools to room temperature afterwards and obtains grey powder target product D1, programming rate 10 degree per minutes; Cooling rate is 5 degree per minutes, promptly obtains the product LiNi of high voltage, high-tap density, high power capacity excellent performance afterwards 0.5Mn 1.5O 4
(7) the pole piece batching (is called for short PVDF according to the ratio of 8:1:1 with active material, acetylene black and binding agent polyvinylidene fluoride; Be dissolved in the 1-Methyl-2-Pyrrolidone) place ball mill mixing stirring ball-milling 3h to apply afterwards, blade thickness is with 150 or 200 microns; The slurry that obtains is coated on the aluminium foil, obtains the grey pole piece, the pole piece after applying is placed 70～80 ℃ the dry 4h of air dry oven, dry compressing tablet, section, weighing pole piece afterwards.Dry by the fire 2-24h down for 120 ℃ at vacuum condition.Subsequently it is transferred to the glove box (water and oxygen content are less than 1 μ molL-1) of argon atmosphere protection; With it is positive pole; Adopt standard C elgard 2700 barrier films between both positive and negative polarity, assembling at last becomes the CR2025 button cell, and electrolyte is 1M LiPF6 EC:DMC=1:1 (v:v).
Fig. 4 is 3.6 V～4.9 V for the high specific energy high power of the lithium ion battery mangaic acid nickel lithium anode material for preparing according to above-mentioned embodiment in the scope of discharging and recharging, the constant current charge-discharge multiplying power be under 1 C first with 200 charging and discharging curves.As can be seen from the figure, circulate first that specific capacity is 122 mAh/g, along with the continuation of circulation; The specific capacity of material is not decay basically, and 200 specific capacities are 119.8mAh/g, capability retention 98%; Enclosed pasture efficient is that 99.5%, 200 time enclosed pasture efficient is 99.5% first.Show that the high specific energy high power mangaic acid nickel lithium anode material that obtains that is synthesized has good cycle life and very high specific capacity, is applicable to suitability for industrialized production;
The lithium ion battery high specific energy high power mangaic acid nickel lithium anode material of Fig. 5 for preparing according to above-mentioned embodiment with the multiplying power of 0.5C, is the first charge-discharge curve under 3.6 V～4.9 V in the scope of discharging and recharging;
The lithium ion battery high specific energy high power mangaic acid nickel lithium anode material of Fig. 6 for preparing according to above-mentioned embodiment with the multiplying power of 0.5C, is 1000 charging and discharging curves under 3.6 V～4.9 V in the scope of discharging and recharging;
The lithium ion battery high specific energy high power mangaic acid nickel lithium anode material XRD figure spectrum of Fig. 7 for preparing according to above-mentioned embodiment.

Claims (10)

1. the present invention provides a kind of high specific energy high power mangaic acid nickel lithium anode material LiNi 0.5Mn 1.5O 4, it is characterized in that having higher tap density, can reach 2.0 ~ 2.5cm 3; And the product particle pattern is regular; Very helping particle surface coats and modifies; For further improving the product chemical property advantageous conditions is provided; Raw material adopts a kind of chelating agent of doing in nickel acetate, manganese acetate, acetate lithium salts and oxalic acid, ammonium oxalate, citric acid, the Triammonium citrate; The presoma that obtains with Prepared by Sol Gel Method makes acetate decompose in 400 ~ 450 ℃ of air, after slight the grinding, in 850 ℃ ~ 900 ℃ oxygen atmospheres, calcines and is annealed to 500 ~ 600 ℃ of calcining 6 ~ 10h after 1 ~ 2h and obtains specimen material.
2. according to claims 1, take by weighing manganese source manganese salt, nickel source nickel salt, lithium source lithium salts respectively by stoichiometric proportion, be mixed with the manganese nickel lithium mixed solution of (Ni+Mn+Li) 0.1525Mol with deionized water dissolving, be labeled as A.
3. according to claims 2, take by weighing chelating agent: a kind of concentration that is mixed with in oxalic acid, ammonium oxalate, citric acid, the Triammonium citrate is 0.15mol solution, is labeled as B.
4. according to claims 2,3, preparation concentration is 25% ammonia spirit.
5. according to claims 2,3, with the solution ultrasonic dissolution or the heating for dissolving that are labeled as A, the solution that is labeled as B is stirred to dissolving under 60 ℃ of states.
6. according to claims 5, the solution that is labeled as B is warming up to 90 ℃ continuing will to be labeled as the A mixed solution again under the stirring, drop in the consoluet B solution; The dropping time is controlled at 30 ~ 60min, and this mixed solution is labeled as C.
7. according to claims 6, to PH=6.5～7.5, be warming up to 90-98 ℃ to the ammoniacal liquor that is labeled as C mixed solution and dripping 25%, be stirred to evaporate to dryness with 3HZ, be the gluey or shallow grass green lump thing of grass green.
8. according to claims 7, will be the presoma of the gluey or shallow grass green lump thing of grass green, in 90 ℃ of vacuumize 12-48h.
9. according to claims 8, presoma moved into place Muffle furnace in the crucible 400-450 ℃ of air preliminary treatment 4-6 hour, 5～10 ℃ of programming rate per minutes are cooled to room temperature naturally.
10. according to claims 9; After products therefrom grinds; In air in 850～900 ℃ of following calcining 1～2h after annealings: 5～10 ℃ of 600～650 ℃ of programming rate per minutes, 5～10 ℃ of cooling rate per minutes, time 8～10h; Naturally after being cooled to room temperature, promptly obtain the product LiNi of high voltage, high-tap density, high power capacity excellent performance 0.5Mn 1.5O 4
CN201210316086XA 2012-08-31 2012-08-31 Preparation method of manganic acid-nickel-lithium positive electrode with high specific energy and high power Pending CN102800856A (en)

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CN103825014A (en) * 2014-01-09 2014-05-28 北京理工大学 Preparation method of lithium ion battery high-voltage cathode material lithium nickel manganese composite oxide
CN107910516A (en) * 2017-11-07 2018-04-13 山东德朗能新能源科技有限公司 A kind of lithium battery high voltage lithium nickel manganese oxygen composite cathode material and its preparation process, lithium battery anode and lithium battery

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CN102491426A (en) * 2011-12-09 2012-06-13 东莞市迈科科技有限公司 Preparation method for lithium battery anode material LiNi0.5Mn1.5O4

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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN103825014A (en) * 2014-01-09 2014-05-28 北京理工大学 Preparation method of lithium ion battery high-voltage cathode material lithium nickel manganese composite oxide
CN103825014B (en) * 2014-01-09 2016-03-02 北京理工大学 A kind of preparation method of high-voltage anode material of lithium ion batteries lithium nickel manganese composite oxide
CN107910516A (en) * 2017-11-07 2018-04-13 山东德朗能新能源科技有限公司 A kind of lithium battery high voltage lithium nickel manganese oxygen composite cathode material and its preparation process, lithium battery anode and lithium battery
CN107910516B (en) * 2017-11-07 2020-12-22 山东德朗能新能源科技有限公司 High-voltage lithium nickel manganese oxide composite positive electrode material for lithium battery, preparation process of high-voltage lithium nickel manganese oxide composite positive electrode material, lithium battery positive electrode and lithium battery

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Application publication date: 20121128