CN102760875B - The preparation method of a kind of ball-shaped lithium-ion battery anode material and presoma thereof - Google Patents

The preparation method of a kind of ball-shaped lithium-ion battery anode material and presoma thereof Download PDF

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CN102760875B
CN102760875B CN201110405938.8A CN201110405938A CN102760875B CN 102760875 B CN102760875 B CN 102760875B CN 201110405938 A CN201110405938 A CN 201110405938A CN 102760875 B CN102760875 B CN 102760875B
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ion battery
nickel
lithium
ball
anode material
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CN102760875A (en
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陈卫华
张建民
米立伟
王爽
姚亚婷
郑文露
孟阵
李绍�
兰梦
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Zhengzhou University
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Abstract

The preparation method of a kind of ball-shaped lithium-ion battery anode material and presoma thereof, freshly prepd nano-sheet nickel hydroxide is made raw material by the method, and be distributed in the aqueous solution, add a certain proportion of cobalt salt wherein, in closed container, a kind of uniform spheric granules can be obtained after stoichiometric number hour can be used as the presoma preparing lithium ion anode material; Then high-temperature calcination after making obtained this granular precursor and lithium salts mix, finally obtains a kind of ball-shaped lithium-ion battery anode material of uniform particle sizes.Method of the present invention is simple to operate, and efficiency is high, and synthesis material is easy to get, and cost is low, environmental protection, and prepared ball-shaped lithium-ion battery anode material chemical property is good.

Description

The preparation method of a kind of ball-shaped lithium-ion battery anode material and presoma thereof
Technical field
The invention belongs to technical field of lithium ion, be specifically related to the preparation method of a kind of ball-shaped lithium-ion battery anode material and presoma thereof.
Background technology
Current, lithium ion battery is the study hotspot of the green traffic instrument power supply system used such as various mobile communication equipment and electric automobile.And the performance of lithium ion battery depends on the performance of its critical material to a great extent, and improved materials performance is a long-term and difficult process.
As the critical active material of lithium ion battery, the shape of its particle directly affects the performance of material.Spherical is the shape of active material the best of commercial cells, and this spherical particle has good mobility, sizing mixing when facilitating pole piece to prepare; In addition, the compactedness of material can also be increased, the bulk density of battery is improved.Current business-like layered oxide lithium ion battery anode material also mainly adopts the material with spherical structure, its preparation method normally co-deposition method obtains the presoma of lithium ion anode material, then obtains having the lithium ion anode material of spheric granules by mixing rear high-temperature calcination with lithium salts.Although this method can, with preparing spherical lithium ion anode material presoma, need strictly to control to ensure the even of material granule to its preparation condition.The present invention there is provided herein a kind of new method preparing spherical layered oxide anode material for lithium-ion batteries and presoma thereof, and the method simply, is easily controlled, and is applicable to large-scale operation, has good application prospect.
Summary of the invention
The object of the present invention is to provide a kind of simple, efficient, new method of being easy to the spherical layered oxide anode material for lithium-ion batteries of preparation and the presoma thereof operated, the specific capacity, cycle performance etc. of the material adopting the method to obtain all can be significantly improved.
The preparation method of ball-shaped lithium-ion battery anode material presoma of the present invention, comprise the steps: that (1) prepares nano-sized nickel hydroxide: by soluble nickel salt with highly basic is soluble in water is respectively mixed with solution, then by soluble nickel salting liquid and strong base solution mixing, mixed liquor is placed in polytetrafluoroethylene reactor in 160-200 DEG C of reaction 8-48 hour, can obtain nano-sized nickel hydroxide after being separated drying; (2) nano-sized nickel hydroxide prepared by step (1) is joined in the middle of the aqueous solution of soluble cobalt, after stirring, be placed in reactor, 2-48 hour is reacted at 120-200 DEG C of temperature, after isolated by filtration at 40-200 DEG C of temperature dry 1-48 hour, namely obtain ball-shaped lithium-ion battery anode material presoma, the diameter of described lithium ion battery material granular precursor is between 1 micron to 30 microns.
Nickel salt used in step (1) is one or more in nickel chloride, nickelous sulfate, nickel nitrate, nickel acetate.
Highly basic used in step (1) is one or more in NaOH, potassium hydroxide, lithium hydroxide.
The molar concentration of step (1) soluble nickel salting liquid is 0.1-2 mol/L, and the molar concentration of strong base solution is 0.1-4 mol/L, and two kinds of solution is that 1:2 ~ 1:2.1 mixes according to the soluble nickel salt contained by wherein with the mol ratio of highly basic.
Soluble cobalt described in step (2) is cobalt chloride, and the concentration of the aqueous solution of soluble cobalt is 0.01 mol/L-5mol/L.
The mol ratio of the nickel comprised in the cobalt comprised in the aqueous solution of the soluble cobalt described in step (2) and nano-sized nickel hydroxide is 0.5:1-6:1.
The preparation method of ball-shaped lithium-ion battery anode material of the present invention, comprise the steps: that (1) prepares nano-sized nickel hydroxide, its concrete steps are: by soluble nickel salt with highly basic is soluble in water is respectively mixed with solution, then by soluble nickel salting liquid and strong base solution mixing, mixed liquor is placed in polytetrafluoroethylene reactor in 160-200 DEG C of reaction 8-48 hour, can obtain nano-sized nickel hydroxide after being separated drying; (2) nano-sized nickel hydroxide prepared by step (1) is joined in the middle of the aqueous solution of soluble cobalt, after stirring, be placed in reactor, 2-48 hour is reacted at 120-200 DEG C of temperature, after isolated by filtration at 40-200 DEG C of temperature dry 1-48 hour, namely obtain the presoma of the uniform lithium ion battery material with spheric granules; (3) calcine respectively at 450-550 DEG C after the presoma of lithium ion battery material step (2) obtained and lithium salts mix and calcine with 650-850 DEG C the ball-shaped lithium-ion battery anode material that 8-24 hour can obtain uniform particle sizes in 4-12 hour.
Nickel salt used in step (1) is one or more in nickel chloride, nickelous sulfate, nickel nitrate, nickel acetate; Highly basic used in step (1) is one or more in NaOH, potassium hydroxide, lithium hydroxide.
Soluble cobalt described in step (2) is cobalt chloride, and the concentration of the aqueous solution of soluble cobalt is 0.01 mol/L-5mol/L; The mol ratio of the nickel comprised in the cobalt comprised in the aqueous solution of the soluble cobalt described in step (2) and nano-sized nickel hydroxide is 0.5:1-6:1.
The particle diameter of described lithium ion battery material is between 1 micron to 30 microns, and its molecular formula is Li xni 1-yco yo 2, 1≤x≤1.3 in formula, 0.1≤y≤0.9.
The electrochemical property test of spherical layered oxide anode material for lithium-ion batteries of the present invention adopts discharge and recharge to test, work electrode adopts plastic-bonded electrode, be lithium sheet to electrode, electrolyte is 1 mol/L LiPF6/EC+DMC (volume ratio 1:1) solution.
The invention has the advantages that and adopt method that is simple, easy, inexpensive, environmental protection to prepare spherical layered oxide anode material for lithium-ion batteries, the preparation for ball-shaped lithium-ion positive electrode provides new method, new approaches.This kind of preparation method is suitable for large-scale operation.Electrochemical results shows, discharge and recharge good reversibility, the cycle performance of this spherical layered oxide anode material for lithium-ion batteries are good.
Accompanying drawing explanation
Fig. 1 a, b are the scanning electron microscope (SEM) photograph of precursor of lithium ionic cell positive material prepared by embodiment 1 and anode material for lithium-ion batteries respectively, illustration in b is the spheric granules enlarged drawing of prepared anode material for lithium-ion batteries, and c is the x-ray spectroscopy figure of prepared anode material for lithium-ion batteries.
The charging and discharging curve figure of the electrode that the anode material for lithium-ion batteries of Fig. 2 prepared by embodiment 1 obtains.
The specific discharge capacity cycle performance figure of the electrode that the anode material for lithium-ion batteries of Fig. 3 prepared by embodiment 1 obtains.
Embodiment
embodiment 1:
prepare nano-sized nickel hydroxide: by the NiCl of 0.015mol 26H 2the NaOH of O, 0.03mol, is dissolved in wiring solution-forming in 25mL water respectively, after both being mixed in reactor, is placed in 180 ° of C baking oven reactions 24 hours, can obtains nano-sized nickel hydroxide after reaction terminates rear separation, drying.
prepare anode material for lithium-ion batteries: be scattered in 50mL distilled water by the nano-sized nickel hydroxide prepared by 0.25 g, and by the CoCl of 2.57 g 26H 2o is dissolved in above-mentioned system, gained mixed liquor is placed in reactor, reacts 24 hours in 200 DEG C of baking ovens, after reaction terminates, naturally cool to room temperature, can obtain the presoma of ball-shaped lithium-ion battery material after centrifugation in 60 DEG C of oven dry, its pattern as shown in fig. ia.As shown in Figure 1, this presoma is spherical particle, and its domain size distribution is comparatively even, is mainly distributed between 8-10 micron.
Get above-mentioned steps and prepare presoma 1 g of the lithium ion battery material of gained and the LiOH ground and mixed of 0.28 g, in Muffle furnace Program to 500 DEG C insulation 5 hours after mixing, calcine 12 hours at 750 DEG C afterwards, naturally can obtain lithium ion battery material (LiNi after cooling 0.19co 0.81o 2), from electromicroscopic photograph shown in Fig. 1 b, this material maintains the pattern of its precursor substantially, and in spherical particle, its domain size distribution is comparatively even, is mainly distributed between 6-10 micron.Obtained material is made into adhered electrode and carries out charge-discharge test, result shows that prepared ball-shaped lithium-ion battery material discharging specific capacity is about 133mAh/g, and discharge curve has higher discharge potential, is mainly distributed between 4.5-3.8V.In addition, the charge-discharge performance of this material is better: within the 1st week to the 2nd week, occur the inducing capacity fading of more about 1%, the specific discharge capacity of the 85th week is about the 2nd week 92%.
embodiment 2:
Nano-sized nickel hydroxide prepared by 0.25 g is scattered in 50mL distilled water, and by the CoCl of 1.93 g 26H 2o is dissolved in above-mentioned system, and gained mixed liquor is placed in reactor, reacts 24 hours in 200 DEG C of baking ovens, naturally cools to room temperature after reaction terminates, and dries the presoma that can obtain ball-shaped lithium-ion battery material after centrifugation in 60 ° of C.
Get above-mentioned steps and prepare presoma 1 g of the lithium ion battery material of gained and the LiOH ground and mixed of 0.28 g, in Muffle furnace Program to 500 DEG C insulation 5 hours after mixing, calcine 12 hours at 750 DEG C afterwards, naturally can obtain ball-shaped lithium-ion battery material (LiNi after cooling 0.23co 0.77o 2).
embodiment 3:
Nano-sized nickel hydroxide prepared by 0.25 g is scattered in 50mL distilled water, and by the CoCl of 1.28 g 26H 2o is dissolved in above-mentioned system, and gained mixed liquor is placed in reactor, reacts 24 hours in 200 DEG C of baking ovens, naturally cools to room temperature, can obtain the presoma of ball-shaped lithium-ion battery material after centrifugation in 60 DEG C of oven dry after reaction terminates.
Get above-mentioned steps and prepare presoma 1 g of the lithium ion battery material of gained and the LiOH ground and mixed of 0.28 g, in Muffle furnace Program to 500 DEG C insulation 5 hours after mixing, calcine 12 hours at 750 DEG C afterwards, naturally can obtain ball-shaped lithium-ion battery material (LiNi after cooling 0.44co 0.56o 2).
embodiment 4:
Nano-sized nickel hydroxide prepared by 0.25 g is scattered in 50mL distilled water, and by the CoCl of 0.64 g 26H 2o is dissolved in above-mentioned system, and gained mixed liquor is placed in reactor, reacts 24 hours in 200 DEG C of baking ovens, naturally cools to room temperature, can obtain the presoma of ball-shaped lithium-ion battery material after centrifugation in 60 DEG C of oven dry after reaction terminates.
Get above-mentioned steps and prepare presoma 1 g of the lithium ion battery material of gained and the LiOH ground and mixed of 0.28 g, in Muffle furnace Program to 500 DEG C insulation 5 hours after mixing, calcine 12 hours at 750 DEG C afterwards, naturally can obtain ball-shaped lithium-ion battery material (LiNi after cooling 0.55co 0.45o 2).
embodiment 5:
Nano-sized nickel hydroxide prepared by 0.25 g is scattered in 50mL distilled water, and by the CoCl of 0.32 g 26H 2o is dissolved in above-mentioned system, and gained mixed liquor is placed in reactor, reacts 24 hours in 200 DEG C of baking ovens, naturally cools to room temperature, can obtain the presoma of ball-shaped lithium-ion battery material after centrifugation in 60 DEG C of oven dry after reaction terminates.
Get above-mentioned steps and prepare presoma 1 g of the lithium ion battery material of gained and the LiOH ground and mixed of 0.28 g, in Muffle furnace Program to 500 DEG C insulation 5 hours after mixing, calcine 12 hours at 750 DEG C afterwards, naturally can obtain ball-shaped lithium-ion battery material (LiNi after cooling 0.61co 0.39o 2).
embodiment 6:
Nano-sized nickel hydroxide prepared by 0.25 g is scattered in 50mL distilled water, and by the CoCl of 0.64 g 26H 2o is dissolved in above-mentioned system, and gained mixed liquor is placed in reactor, reacts 8 hours in 200 DEG C of baking ovens, naturally cools to room temperature, can obtain the presoma of ball-shaped lithium-ion battery material after centrifugation in 60 DEG C of oven dry after reaction terminates.
Get above-mentioned steps and prepare presoma 1 g of the lithium ion battery material of gained and the LiOH ground and mixed of 0.28 g, in Muffle furnace Program to 500 DEG C insulation 5 hours after mixing, calcine 12 hours at 750 DEG C afterwards, naturally can obtain ball-shaped lithium-ion battery material (LiNi after cooling 0.35co 0.65o 2).
embodiment 7:
Nano-sized nickel hydroxide prepared by 1 g is scattered in 50mL distilled water, and by the CoCl of 5 g 26H 2o is dissolved in above-mentioned system, gained mixed liquor is placed in reactor, reacts 24 hours in 200 DEG C of baking ovens, after reaction terminates, naturally cool to room temperature, dry the presoma that can obtain ball-shaped lithium-ion battery material after centrifugation in 60 ° of C, its pattern as shown in Figure 1 b.
Get above-mentioned steps and prepare presoma 1 g of the lithium ion battery material of gained and the LiOH ground and mixed of 0.28 g, in Muffle furnace Program to 500 DEG C insulation 5 hours after mixing, calcine 12 hours at 750 DEG C afterwards, naturally can obtain ball-shaped lithium-ion battery material (LiNi after cooling 0.36co 0.64o 2).

Claims (6)

1. the preparation method of a ball-shaped lithium-ion battery anode material presoma, (1) prepares nano-sized nickel hydroxide to it is characterized in that the method comprises the steps:: by soluble nickel salt with highly basic is soluble in water is respectively mixed with solution, then by soluble nickel salting liquid and strong base solution mixing, mixed liquor is placed in polytetrafluoroethylene reactor in 160-200 DEG C of reaction 8-48 hour, can obtain nano-sized nickel hydroxide after being separated drying; (2) nano-sized nickel hydroxide prepared by step (1) is joined in the middle of the aqueous solution of cobalt chloride, the concentration of cobalt chloride solution is 0.01 mol/L-5mol/L, after stirring, be placed in reactor, 2-48 hour is reacted at 120-200 DEG C of temperature, after isolated by filtration at 40-200 DEG C of temperature dry 1-48 hour, namely obtain ball-shaped lithium-ion battery anode material presoma;
The molar concentration of step (1) soluble nickel salting liquid is 0.1-2 mol/L, and the molar concentration of strong base solution is 0.1-4 mol/L, and two kinds of solution is that 1:2 ~ 1:2.1 mixes according to the soluble nickel salt contained by wherein with the mol ratio of highly basic;
The mol ratio of the nickel comprised in the cobalt comprised in the aqueous solution of the cobalt chloride described in step (2) and nano-sized nickel hydroxide is 0.5:1-6:1.
2. the preparation method of ball-shaped lithium-ion battery anode material presoma according to claim 1, is characterized in that: nickel salt used in step (1) is one or more in nickel chloride, nickelous sulfate, nickel nitrate, nickel acetate.
3. the preparation method of ball-shaped lithium-ion battery anode material presoma according to claim 1, is characterized in that: highly basic used in step (1) is one or more in NaOH, potassium hydroxide, lithium hydroxide.
4. the preparation method of a ball-shaped lithium-ion battery anode material, (1) prepares nano-sized nickel hydroxide to it is characterized in that the method comprises the steps:, its concrete steps are: by soluble nickel salt with highly basic is soluble in water is respectively mixed with solution, then by soluble nickel salting liquid and strong base solution mixing, mixed liquor is placed in polytetrafluoroethylene reactor in 160-200 DEG C of reaction 8-48 hour, can obtain nano-sized nickel hydroxide after being separated drying; (2) nano-sized nickel hydroxide prepared by step (1) is joined in the middle of the aqueous solution of soluble cobalt, after stirring, be placed in reactor, 2-48 hour is reacted at 120-200 DEG C of temperature, after isolated by filtration at 40-200 DEG C of temperature dry 1-48 hour, namely obtain the presoma of the uniform lithium ion battery material with spheric granules; (3) calcine respectively at 450-550 DEG C after the presoma of lithium ion battery material step (2) obtained and lithium salts mix and calcine with 650-850 DEG C the ball-shaped lithium-ion battery anode material that 8-24 hour can obtain uniform particle sizes in 4-12 hour;
Soluble cobalt described in step (2) is cobalt chloride, and the concentration of the aqueous solution of soluble cobalt is 0.01 mol/L-5mol/L; The mol ratio of the nickel comprised in the cobalt comprised in the aqueous solution of the soluble cobalt described in step (2) and nano-sized nickel hydroxide is 0.5:1-6:1.
5. the preparation method of ball-shaped lithium-ion battery anode material according to claim 4, is characterized in that: nickel salt used in step (1) is one or more in nickel chloride, nickelous sulfate, nickel nitrate, nickel acetate; Highly basic used in step (1) is one or more in NaOH, potassium hydroxide, lithium hydroxide.
6. the preparation method of ball-shaped lithium-ion battery anode material according to claim 4, is characterized in that: the particle diameter of described lithium ion battery material is between 1 micron to 30 microns, and its molecular formula is Li xni 1-yco yo 2, 1≤x≤1.3 in formula, 0.1≤y≤0.9.
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