CN102306760A - Preparation method of lithium ion battery positive electrode composite material and precursor thereof - Google Patents
Preparation method of lithium ion battery positive electrode composite material and precursor thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a lithium ion battery positive electrode composite material and a precursor thereof, and in particular relates to a novel method for preparing a high-purity low-cost binary or ternary precursor and preparing a high-performance lithium ion battery binary or ternary positive electrode composite material by utilizing the precursor, belonging to the technical field of new energy materials and the preparation thereof. The method comprises the following specific steps: (1) putting salt-type solid raw materials of two or three of nickel, cobalt and manganese with crystal water into a reactor, and heating the materials to the molten state; (2) introducing ammonia under the protection of inert gas, supplementing a small amount of water or no water according to the solubility of salts at different temperatures, stirring and reacting; (3) evaporating ammonium salt after full reaction, taking the solid out, and drying so as to get the amorphous binary or ternary positive electrode composite material precursor; and (4) mixing the precursor with lithium carbonate according to a certain ratio, and further preparing the lithium ion battery positive electrode composite material through a two-section sintering method. The precursor synthetic method is simple, sodium hydroxide is avoided from being used, separation and purification are not required, and the high-purity positive electrode composite material precursor which has no impurities basically can be obtained; furthermore, no industrial waste water is discharged, and the by-product ammonium salt can further generate economic benefit; and the positive electrode composite material prepared by the precursor has excellent performances, and is convenient for industrialization.
Description
Technical field
The present invention relates to a kind of method for preparing anode composite material of lithium ion battery; Relate in particular to high-purity low-cost binary of a kind of preparation or ternary precursor; Reach the method for preparing high performance lithium ion battery binary or tertiary cathode composite material by this precursor, belong to new energy materials and preparing technical field.
Background technology
During the nearly last ten years, lithium ion battery has obtained extensive use and has occupied leading position in telecommunications fields such as mobile phone, notebook computer, video cameras.Represent the new-energy automobile of following automobile industry developing direction, its major impetus comprises lithium ion battery, and the new-energy automobile industrialization will directly drive lithium ion battery market and increase fast.China's automobile every year, the speed with 15% increased, and electric automobile is the main force of following automobile as the emphasis of new-energy automobile development.But the lithium battery as the source of power is a restriction electric automobile development key factor, accounts for more than 50% of whole electric motor car cost at present.Therefore, the reduction of integral vehicle cost depends on the reduction of lithium battery production cost to a great extent.
Lithium ion battery is made up of positive pole, negative pole, electrolyte, barrier film four big critical materials, and positive electrode accounts for 1/3rd of lithium ion battery production prices.Therefore, the reduction of positive electrode cost is the key that influences lithium ion battery and even electric automobile price.
The commodity anode material for lithium-ion batteries mainly contains cobalt acid lithium, LiMn2O4, the binary of nickel, cobalt, manganese or ternary material, LiFePO4 at present.Wherein binary or ternary material are because its distinctive advantage (promptly combines LiCoO
2, LiNiO
2, LiMnO
2The advantage of stratified material, its performance are superior to above arbitrary one-component positive electrode, and cobalt acid lithium cost is low relatively; Safe; The LiMn2O4 capacity is high relatively, and high temperature cyclic performance is good, and the LiFePO4 discharge platform is high relatively; Capacity is high, and is can force density big) the dynamic lithium battery field and cause showing great attention to of people especially in the lithium battery field.
The binary of bibliographical information or the synthetic method of tertiary cathode composite material have high temperature solid-state method, sol-gal process, spray drying process etc. at present.High temperature solid-state method is simple because of its equipment and technology; Preparation condition is easy to control; Be the main method of present large-scale production binary or tertiary cathode composite material, like Chinese publication " CN1843930A " " CN101510602A " " CN1964103A " " CN1622371A " etc.Adopting NaOH or carbonate in these patents is precipitation reagent, and at first synthetic binary or ternary precursor heats one with the lithium source again and go on foot and obtain binary or tertiary cathode material under hot conditions.But there is following shortcoming in the anode composite material by these methods obtain: product purity is lower, and especially sodium content exceeds standard, and has a strong impact on the performance of battery performance; The synthesis technique step is more relatively, and the accessory substance utilance is not high, causes production cost higher; Industrial wastewater is more in the building-up process, or does not reach environmental protection requirement or the like.Therefore, high temperature solid-state method production anode composite material of lithium ion battery method haves much room for improvement and improves, to satisfy the requirement to anodal composite material quality and output of ever-increasing plain edition lithium battery and new forms of energy dynamic lithium battery.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of lithium ion battery binary or tertiary cathode composite material precursor; Shortened process greatly; Improve lithium ion battery binary or the purity of tertiary cathode composite material and the utilance of product, reduce the pollution of accessory substance environment.
Another object of the present invention aims to provide the method for utilizing lithium ion battery binary that said method makes or tertiary cathode composite material precursor to obtain the anode composite material of high performance-price ratio.
The technical scheme of the preparation of lithium ion battery binary of the present invention or tertiary cathode composite material precursor may further comprise the steps:
The solid salt that (1) will have nickel, cobalt, manganese any two or three kinds of the crystallization water is put into reactor, is heated to molten state;
(2) under inert gas argon gas or nitrogen protection, feed ammonia; Suitably replenish low amounts of water or do not add water in the solubility under the different temperatures (solid salt self crystallization water then needs supplementing water as not forming saturated solution under this temperature) according to the solid salt that is adopted, reaction while stirring;
Treat that (3) (2) step steams ammonium salt after reacting completely through distillation, take out solid, oven dry obtains amorphous binary or tertiary cathode composite material precursor.
The said salt solid material that has nickel, cobalt or the manganese of the crystallization water is preferably hydration nickel chloride, hydrated cobalt chloride or hydration manganese chloride.
In said (1) step, heating and temperature control is between 85~120 ℃.
Described (2) ammonia flow is controlled at 0.02~0.08L/min, is convenient to controls reaction speed, improves productive rate.
The temperature that said (3) in the step steam ammonium salt is controlled at 335~370 ℃.
Adopt in the still-process in said (3) step and use water as circulating coolant.
The ammonium chloride that adopts water absorbing hydrogen chloride and ammonia in said (3) step or distil out is convenient to reclaim accessory substance, improves the product surcharge.
The preparation of lithium ion battery binary of the present invention or tertiary cathode composite material is: the described precursor that adopts above method to make mixes with lithium carbonate; Batch mixing is even in ball mill, divides double sintering can prepare the high performance lithium ion battery anode composite material.
Preferred version is: described precursor and lithium salts mol ratio are 1: 11~1.24.
Described double sintering is: first section sintering temperature is controlled at 500~600 ℃, and sintering time is 3~6h, after sintering finishes, grinds, sieve; Carry out second section high temperature sintering again, its sintering temperature is controlled at 850~1100 ℃, and sintering time is 8~18h.
The present invention has at first invented a kind of high-purity, low-cost, easy to operate, zero new method of polluting preparation lithium ion battery amorphous binary or ternary precursor; Promptly adopting the low-cost nickel that has a crystallization water, cobalt, manganese any two or three kinds of salt solids is raw material; Under molten condition and ammonia react, heating steams the salt solid and can obtain high-purity amorphous binary or ternary precursor.
The present invention provides a kind of method for preparing high-crystallinity bulky grain anode composite material then, and promptly adopting indefiniteness binary or ternary precursor and lithium carbonate is raw material, divides the double sintering method can prepare the high-performance anode composite material.
Several kinds of salt solid materials of nickel, cobalt, manganese and ammonia react that the present invention adopts the solid fusion method will have the crystallization water first obtain binary or ternary precursor, and are the synthetic bulky grain high-performance anode composite material of raw material with precursor and lithium carbonate.Wherein, the LiNi that obtains by above method
1/3Co
1/3Mn
1/3O
2The ternary material tap density reaches 2.35g/cm
3More than, discharge capacity is up to 156mAh/g first under the button cell 2C multiplying power of assembling, and 30 times the above capacity that circulates remains on more than 93%.
This precursor synthetic method is simple, and cost of material is cheap, and technological process is short, is convenient to operation, and synthetic, separation and purification one kettle way just can obtain binary or ternary precursor; Avoid the use of NaOH, thereby saved washing step, need not to separate and purify, can obtain the binary or the ternary precursor of high-purity substantially free of impurities; And do not have industrial wastewater discharge, by-product ammonium chloride also can produce economic worth.By the anode composite material excellent performance that this precursor prepares, low price is convenient to industrialization.
Description of drawings
Fig. 1 is for preparing the XRD figure of sample according to embodiment 1 method;
Fig. 2 is for preparing the SEM figure of sample according to embodiment 1 method;
Fig. 3 is for to prepare sample cycle performance figure under the 2C multiplying power according to embodiment 1 method.
Embodiment
Following examples are intended to explain the present invention rather than to further qualification of the present invention.The preparation embodiment of binary material please be provided in addition.
Embodiment 1
(1) be in molar ratio take by weighing at 1: 1: 1 hydration nickel chloride, hydrated cobalt chloride, hydration manganese chloride altogether 100g put into reactor, be heated to 90 ℃;
(2) under inert gas argon gas or nitrogen protection, feed liquefied ammonia, replenish 62.7g water, slowly add by dropping funel, reaction while stirring, the liquefied ammonia flow is controlled at 0.04L/min;
(3) question response changes after fully and makees distilling apparatus, adopts in the distilling apparatus and uses water as circulating coolant, and the gas receiving system adopts water absorbing hydrogen chloride and ammonia.The electric jacket heating, temperature is controlled at 340 ℃, and ammonium salt is steamed, and takes out solid, and oven dry obtains amorphous tertiary cathode material precursor.
(4) with precursor and lithium carbonate be 1: 1: 1 mixed by metal ion and lithium ion mol ratio; Batch mixing is even in planetary ball mill; 500 ℃ of following sintering 4h in Muffle furnace grind, and 200 orders sieve; Again muffle furnace is controlled at 1100 ℃, sintering 10h can obtain high performance tertiary cathode material.Grain size analysis shows that D50 is 9.4 μ m, and its tap density reaches 2.42g/cm
3, Na
+Content is merely 31ppm, and other impurity has all reached the requirement of commercially available tertiary cathode material.
(5) be anodal with the tertiary cathode material, the lithium sheet is a negative pole, and the assembling button cell carries out electrochemical property test discharging and recharging on the appearance.Initial discharge capacity is 155mAh/g under the 2C multiplying power, circulates after 50 times, and capability retention is 93%.
(1) be in molar ratio take by weighing at 1: 1: 1 hydration nickel chloride, hydrated cobalt chloride, hydration manganese chloride altogether 100g put into three-neck flask, be heated to 120 ℃;
(2) under inert gas argon gas or nitrogen protection, feed liquefied ammonia, reaction while stirring, the liquefied ammonia flow is controlled at 0.08L/min;
(3) question response changes after fully and makees distilling apparatus, adopts in the distilling apparatus and uses water as circulating coolant, and the gas receiving system adopts water absorbing hydrogen chloride and ammonia.The electric jacket heating, temperature is controlled at 360 ℃, and ammonium salt is steamed, and takes out solid, and oven dry obtains amorphous tertiary cathode material precursor.
(4) with precursor and lithium carbonate be 1: 118 mixed by metal ion and lithium ion mol ratio; Batch mixing is even in planetary ball mill; 450 ℃ of following sintering 3h in Muffle furnace grind, and 200 orders sieve; Again muffle furnace is controlled at 1050 ℃, sintering 14h can obtain high performance tertiary cathode material.Grain size analysis shows that D50 is 8.9 μ m, and its tap density reaches 2.35g/cm
3, Na
+Content is merely 15ppm, and other impurity has all reached the requirement of commercially available tertiary cathode material.
(5) be anodal with the tertiary cathode material, the lithium sheet is a negative pole, and the assembling button cell carries out electrochemical property test discharging and recharging on the appearance.Initial discharge capacity is 156mAh/g under the 2C multiplying power, circulates after 40 times, and capability retention is 95%.
Embodiment 3
(1) be in molar ratio take by weighing at 1: 1: 1 hydration nickel chloride, hydrated cobalt chloride, hydration manganese chloride altogether 100g put into three-neck flask, be heated to 110 ℃;
(2) under inert gas argon gas or nitrogen protection, feed liquefied ammonia, reaction while stirring, the liquefied ammonia flow is controlled at 0.05L/min.
(3) question response changes after fully and makees distilling apparatus, adopts in the distilling apparatus and uses water as circulating coolant, and the gas receiving system adopts water to absorb ammonium chloride.The electric jacket heating, temperature is controlled at 355 ℃, and ammonium salt is steamed, and takes out solid, and oven dry obtains amorphous tertiary cathode material precursor.
(4) with precursor and lithium carbonate be 1: 1.22 mixed by metal ion and lithium ion mol ratio; Batch mixing is even in planetary ball mill; 500 ℃ of following sintering 5h in Muffle furnace grind, and 200 orders sieve; Again muffle furnace is controlled at 950 ℃, sintering 12h can obtain high performance tertiary cathode material.Grain size analysis shows that D50 is 9.1 μ m, and its tap density reaches 2.39g/cm
3, Na
+Content is merely 28ppm, and other impurity has all reached the requirement of commercially available tertiary cathode material.
(5) be anodal with the tertiary cathode material, the lithium sheet is a negative pole, and the assembling button cell carries out electrochemical property test discharging and recharging on the appearance.Initial discharge capacity is 158mAh/g under the 2C multiplying power, circulates after 50 times, and capability retention is 94.6%.
Embodiment 4
(1) be in molar ratio take by weighing at 5: 3: 2 hydration nickel chloride, hydration manganese chloride, hydrated cobalt chloride altogether 100g put into three-neck flask, be heated to 105 ℃;
(2) under inert gas argon gas or nitrogen protection, feed liquefied ammonia, reaction while stirring, the liquefied ammonia flow is controlled at 0.05L/min;
(3) question response changes after fully and makees distilling apparatus, adopts in the distilling apparatus and uses water as circulating coolant, and the gas receiving system adopts water to absorb ammonium chloride.The electric jacket heating, temperature is controlled at 370 ℃, and ammonium salt is steamed, and takes out solid, and oven dry obtains amorphous tertiary cathode material precursor.
(4) with precursor and lithium carbonate be 1: 1.2 mixed by metal ion and lithium ion mol ratio; Batch mixing is even in planetary ball mill; 550 ℃ of following sintering 4h in Muffle furnace grind, and 200 orders sieve; Again muffle furnace is controlled at 900 ℃, sintering 16h can obtain high performance tertiary cathode material.Grain size analysis shows that D50 is 9.3 μ m, and its tap density reaches 2.43g/cm
3, Na
+Content is merely 21ppm, and other impurity has all reached the requirement of commercially available tertiary cathode material.
(5) be anodal with the tertiary cathode material, the lithium sheet is a negative pole, and the assembling button cell carries out electrochemical property test discharging and recharging on the appearance.Initial discharge capacity is 162mAh/g under the 2C multiplying power, circulates after 50 times, and capability retention is 93.8%.
(1) be in molar ratio take by weighing at 1: 1 hydration nickel chloride, hydration manganese chloride altogether 100g put into three-neck flask, be heated to 90 ℃;
(2) under inert gas argon gas or nitrogen protection, feed liquefied ammonia, reaction while stirring, the liquefied ammonia flow is controlled at 0.06L/min;
(3) question response changes after fully and makees distilling apparatus, adopts in the distilling apparatus and uses water as circulating coolant, and the gas receiving system adopts water to absorb ammonium chloride.The electric jacket heating, temperature is controlled at 360 ℃, and ammonium salt is steamed, and takes out solid, and oven dry obtains the amorphous binary anode material precursor.
(4) with precursor and lithium carbonate be 1: 115 mixed by metal ion and lithium ion mol ratio; Batch mixing is even in planetary ball mill; 550 ℃ of following sintering 4h in Muffle furnace grind, and 200 orders sieve; Again muffle furnace is controlled at 900 ℃, sintering 15h can obtain high performance binary positive electrode.
(5) be positive pole with the binary positive electrode, the lithium sheet is a negative pole, and the assembling button cell carries out electrochemical property test discharging and recharging on the appearance.Initial discharge capacity is 164.4mAh/g under the 2C multiplying power, circulates after 30 times, and capability retention is 94%.
Claims (10)
1. the preparation method of an anode composite material of lithium ion battery precursor is characterized in that, may further comprise the steps:
Any two or three kinds that (1) will have in the solid salt of nickel, cobalt, manganese of the crystallization water are put into reactor, are heated to molten state;
(2) under inert gas shielding, feed ammonia, suitably replenish low amounts of water or do not add water according to the solubility of the solid salt that is adopted under different temperatures, the solid salt that is promptly adopted self crystallization water then needs supplementing water as not forming saturated solution under this temperature; Reaction while stirring;
Treat that (3) (2) step steams ammonium salt after reacting completely through distillation, take out solid, oven dry obtains amorphous anode composite material of lithium ion battery precursor.
2. the preparation method of precursor according to claim 1 is characterized in that, ammonia flow is controlled at 0.02~0.08L/min in the step (2).
3. the preparation method of precursor according to claim 1 is characterized in that ammonium salt described in the step (3) steams temperature and is controlled at 335~370 ℃.
4. the preparation method of precursor according to claim 1 is characterized in that, step (1) in the step heating and temperature control between 85~120 ℃.
5. the preparation method of precursor according to claim 1 is characterized in that, adopts in the still-process in said (3) step and uses water as circulating coolant, hydrogen chloride that adopts water to absorb to distill out and ammonia or the ammonium chloride that distils out.
6. the preparation method of precursor according to claim 1 is characterized in that the solid salt that has nickel, cobalt or the manganese of the crystallization water described in the step (1) is hydration nickel chloride, hydrated cobalt chloride or hydration manganese chloride.
7. the preparation method of precursor according to claim 1 is characterized in that, described in the step (1) in any two solid salts of nickel, manganese, cobalt two metal ion species mol ratios be 1: 1; Three metal ion species mol ratios are 1: 1: 1 or 5: 3: 2 in the solid salt of nickel, manganese and cobalt.
8. the preparation method of anode composite material of lithium ion battery adopts each method lithium ion cell prepared anode composite material precursor of claim 1-7 to mix with lithium carbonate, divides double sintering to get final product.
9. preparation method as claimed in claim 8 is characterized in that, said precursor and lithium salts mol ratio are 1: 1.08~1: 1.24.
10. preparation method as claimed in claim 9 is characterized in that, said double sintering is: first section sintering temperature is controlled at 500~600 ℃, and sintering time is 3~6h; After first section sintering finishes, grind, 200 orders sieve; Second section sintering temperature is controlled at 850~1100 ℃, and sintering time is 8~18h.
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Cited By (2)
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CN105633397A (en) * | 2015-12-31 | 2016-06-01 | 常州市长宇实用气体有限公司 | Preparation method of lithium manganese nickel oxide-doped refined material |
CN107706370A (en) * | 2017-09-10 | 2018-02-16 | 绵阳梨坪科技有限公司 | A kind of anode composite material of lithium ion battery forerunner's preparation of simple process |
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CN107706370A (en) * | 2017-09-10 | 2018-02-16 | 绵阳梨坪科技有限公司 | A kind of anode composite material of lithium ion battery forerunner's preparation of simple process |
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