CN102315429A - Preparation method of aluminum-doped material of cathode of lithium ion battery with solid phase process - Google Patents
Preparation method of aluminum-doped material of cathode of lithium ion battery with solid phase process Download PDFInfo
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- CN102315429A CN102315429A CN201110222403A CN201110222403A CN102315429A CN 102315429 A CN102315429 A CN 102315429A CN 201110222403 A CN201110222403 A CN 201110222403A CN 201110222403 A CN201110222403 A CN 201110222403A CN 102315429 A CN102315429 A CN 102315429A
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Abstract
The invention relates to a preparation method of an aluminum-doped material of a cathode of a lithium ion battery with a solid phase process. The preparation method comprises the following steps: controlling certain reaction conditions to prepare a precursor of a nickel, cobalt and/or manganese hydroxide; uniformly mixing the precursor with a lithium salt and a nanometer aluminum compound; and carrying out high temperature processing for a certain period of time in an air or oxygen atmosphere, cooling, and crushing to obtain the aluminum-doped material of the cathode of the lithium ion battery with the solid phase process. The aluminum-doped material of the cathode of the lithium ion battery with the solid phase process which can substantially improve the safety performance and the cycle characteristic of the lithium ion battery at a high temperature can be applied to power batteries.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries, relate in particular to the preparation method of lithium ion battery anode material doped aluminium.
Background technology
During the lithium ion battery of being used widely at present, its positive electrode are just experiencing constantly renewal and are improveing.Anode material for lithium-ion batteries has a lot of systems, is used for the lithium and cobalt oxides series (LiCoO that mainly contains stratiform of practical application at present
2), the lithium nickel oxide of stratiform series (LiNiO
2) and the lithium manganese oxide of spinelle shape series (LiMn
2O
4).But above-mentioned system all exists apparent deficiency, has influenced their practical application.The polynary electrode material of nickle cobalt lithium manganate is that the new type lithium ion battery that development in recent years is got up is used positive electrode, and it has concentrated LiCoO
2, LiNiO
2And LiMnO
2The advantage of three kinds of materials has received the researcher and has paid close attention to widely.Because of having replaced the cobalt of 2/3rds (or more) in the sour lithium of cobalt with relatively inexpensive nickel and manganese, so its cost aspect has clear superiority, and simultaneously, its reversible capacity is big, Stability Analysis of Structures, and security performance is good, have higher conductivity and thermal stability.
At present, the preparation method of nickel-cobalt lithium manganate material mainly adopts high temperature solid phase synthesis, coprecipitation.Wherein high temperature solid phase synthesis with lithium source, nickel source, cobalt source and manganese source ground and mixed, is calcined under 1000 ℃ of left and right sides high temperature and is synthesized, and forms through fine grinding at last.This method weak point is: the one, and solid-state diffusion speed is slow, and batch mixing is difficult to evenly, and product exists than big-difference at aspects such as structure, compositions, thereby causes its chemical property wayward; The 2nd, the powder body material bulk density of synthesizing is low, and the tap density of generally accomplishing is merely 1.6~1.8g/cm
3, the volume and capacity ratio that makes nickle cobalt lithium manganate is affected its practical application than low of the sour lithium of cobalt more.And coprecipitation prepares the preparation that the nickle cobalt lithium manganate technical process mainly is a presoma, mixed lithium and sintering; The co-precipitation from the soluble metal salting liquid of general elder generation goes out the presoma of hydroxide, carbonate or the oxide of nickel and cobalt containing manganese; Then presoma filter, wash, after dry back adopts the solid phase mixing mode to mix with lithium salts; At high temperature sintering obtains nickle cobalt lithium manganate.
But pure nickle cobalt lithium manganate ternary material is only applicable to general battery at present, and high temperature safe performance and high temperature cyclic performance are not fine.
Summary of the invention
Technical problem to be solved by this invention is: overcome the deficiency of prior art, provide a kind of be used for anode material for lithium-ion batteries solid phase method adulterated al electrokinetic cell, that have high temperature safe performance and cycle characteristics preferably the preparation method.
For solving the problems of the technologies described above, the technical scheme that the present invention takes is:
A kind of preparation method of anode material for lithium-ion batteries solid phase method adulterated al, its step comprises: at first producing structural formula is Ni
xCo
yMn
z(OH)
2The granular precursor of (x+y+z=1,0≤x≤1,0≤y≤1,0≤z≤1), washing, drying obtains the hydroxide presoma; Said presoma and lithium salts, nanometer aluminum compound is even, and through high-temperature process, cooling is pulverized, and promptly obtains the anode material for lithium-ion batteries of solid phase adulterated al element in air or oxygen, and concrete steps comprise:
(1) produce nickel, cobalt and/or manganese hydroxide presoma:
To contain soluble nickel salt, cobalt salt and manganese salt, or nickel salt and cobalt salt, or nickel salt and manganese salt, one of perhaps said three kinds of salt carry out precipitation reaction with the sodium hydroxide solution that is mixed with ammoniacal liquor, and the formation structural formula is Ni
xCo
yMn
z(OH)
2The granular precursor of (x+y+z=1,0≤x≤1,0≤y≤1,0≤z≤1), washing, drying obtains nickel, cobalt and/or manganese hydroxide presoma;
(2) adulterated al element:
To go up the resulting nickel of step, cobalt and/or manganese hydroxide presoma and nanometer aluminum compound mol ratio by Al/D=0.01~0.05, with the lithium salts mol ratio by Li/ (D+Al)=1.0~1.2; Mix; Make it to mix; Said D=Ni+Co+Mn or Ni+Co, Ni+Mn or Mn+Co, or Ni, Co, Mn any;
(3) high-temperature process:
The mixture of last step gained is carried out high-temperature process, and cooling is then pulverized, and sieves and promptly obtains the anode material for lithium-ion batteries of adulterated al element.
Said nanometer aluminum compound is aluminium isopropoxide, aluminium oxide or aluminium hydroxide.Preferred aluminium isopropoxide.
Said nickel salt, cobalt salt or manganese salt, adopt sulfate, chlorate, nitrate wherein one or more.
Said lithium salts, adopt lithium carbonate, monohydrate lithium hydroxide, lithium nitrate wherein one or more.
The present invention also provides a kind of anode material for lithium-ion batteries, and this anode material for lithium-ion batteries is to make according to aforementioned preparation method.
The invention has the advantages that:
1), solid phase method directly mixes, than before the simple and convenient operation of method that coats of precursor, saved steps such as being configured to slurry, technical process is simple and easy to operate, can make that manufacturing cost reduces, controllable product quality property is better.
2), the doping process adopts the nanoscale aluminium isopropoxide because aluminium content is lower in this material, the dopant material large usage quantity reaches during mixing than high evenness easily, adopts very even that the method for ball milling can mix.
Brief Description Of Drawings:
Fig. 1 is the high temperature cyclic performance curve comparison diagram of the lithium ion battery made of the anode material for lithium-ion batteries of embodiment 1 and Comparative Examples, and wherein, A represents embodiment 1, and B represents Comparative Examples.
Fig. 2 is the Electronic Speculum figure of embodiment 1 gained anode material for lithium-ion batteries.
Fig. 3 is the X-ray energy dispersion spectrogram of embodiment 1 gained anode material for lithium-ion batteries.
Embodiment:
Below in conjunction with specific embodiment the present invention is done further elaboration.
Embodiment 1:
With NiSO
4, CoSO
4, MnSO
4Ni in molar ratio
2+: CO
2+: Mn
2+=4: 2: 4 mixed, use deionized water dissolving, be made into the solution that comprehensive ion concentration is 2mol/L.The sodium hydroxide solution of preparation 4mol/L, and in sodium hydroxide solution, allocate NH into
3H
2The ammoniacal liquor of O: NaOH=0.2.In the parallel adding of two kinds of mixed solutions agitated reactor, under the protection of nitrogen or inert gas, control reaction with the mode of successive reaction, between the pH value control 10-12, temperature 50-60 ℃, filtration washing to wash water pH value 120 ℃ of oven dry down, promptly gets Ni less than 8
0.4Co
0.2Mn
0.4(OH)
2Presoma.
According to Al/ (Ni+Mn+Co)=0.02, Li/ (Ni+Co+Mn+Al)=1.05 molar ratio weighing nanoscale aluminium isopropoxide, lithium carbonate and the presoma of having made evenly mixed 4 hours; The material that mixes is put into sintering furnace carry out sintering; In air atmosphere, be incubated 10 hours down at 900 ℃~1050 ℃, be cooled to room temperature naturally; Crushing and classification obtains containing the nickle cobalt lithium manganate tertiary cathode material of aluminium.
Present embodiment 1 is as shown in Figure 1 with the battery high-temperature cyclic curve comparison diagram of Comparative Examples.
The Electronic Speculum figure of present embodiment gained nickle cobalt lithium manganate positive electrode is as shown in Figure 2.
The x-ray photoelectron ability spectrogram of gained nickle cobalt lithium manganate positive electrode is as shown in Figure 3.
Comparative Examples:
With NiSO
4, CoSO
4, MnSO
4Ni in molar ratio
2+: CO
2+: Mn
2+=4: 2: 4 mixed, use deionized water dissolving, be made into the solution that comprehensive ion concentration is 2mol/L.The sodium hydroxide solution of preparation 4mol/L, and in sodium hydroxide solution, allocate NH into
3H
2The ammoniacal liquor of O: NaOH=0.2.Add in the agitated reactor two kinds of mixed solutions are parallel, under the protection of nitrogen or inert gas, control reaction with the mode of successive reaction, between the pH value control 10-12, temperature 50-60 ℃, filtration washing to wash water pH value 120 ℃ of oven dry down, promptly gets Ni less than 8
0.4Co
0.2Mn
0.4(OH)
2Presoma.
According to mol ratio Li/ (Ni+Co+Mn)=1.05 weighing lithium carbonate and presoma; Evenly mixed 4 hours, the material that mixes is put into sintering furnace carry out sintering, in air; Be incubated 10 hours down at 900 ℃~1050 ℃; Naturally be cooled to room temperature, crushing and classification obtains the not tertiary cathode material of metallized aluminum.
The contrast of battery high-temperature cyclic curve is as shown in Figure 1.
Embodiment 2:
With NiCl
2, CoCl
2, MnCl
2Ni in molar ratio
2+: CO
2+: Mn
2+=70: 15: 15 mixed, use deionized water dissolving, be made into the solution that comprehensive ion concentration is 2mol/L.The sodium hydroxide solution of preparation 4mol/L, and in sodium hydroxide solution, allocate NH into
3H
2The ammoniacal liquor of O: NaOH=0.2.Add in the agitated reactor two kinds of mixed solutions are parallel, under the protection of nitrogen or inert gas, control reaction with the mode of successive reaction, between the pH value control 10-12, temperature 50-60 ℃, filtration washing to wash water pH value 120 ℃ of oven dry down, promptly gets Ni less than 8
0.7Co
0.15Mn
0.15(OH)
2Presoma.
According to Al/ (Ni+Mn+Co)=0.02, Li/ (Ni+Co+Mn+Al)=1.15 molar ratio weighing nanoscale aluminium isopropoxide, lithium carbonate and the presoma of having made evenly mixed 4 hours; The material that mixes is put into sintering furnace carry out sintering; In oxygen atmosphere, be incubated 10 hours down at 900 ℃~1050 ℃, be cooled to room temperature naturally; Crushing and classification obtains containing the nickle cobalt lithium manganate tertiary cathode material of aluminium.
Claims (3)
1. the preparation method of an anode material for lithium-ion batteries solid phase method adulterated al, it is characterized in that: at first producing structural formula is Ni
xCo
yMn
z(OH)
2The granular precursor of (x+y+z=1,0≤x≤1,0≤y≤1,0≤z≤1), washing, drying obtains the hydroxide presoma; Said presoma and lithium salts, nanometer aluminum compound is even, and through high-temperature process, cooling is pulverized, and promptly obtains the anode material for lithium-ion batteries of solid phase adulterated al element in air or oxygen, and concrete steps comprise:
(1) produce nickel, cobalt and/or manganese hydroxide presoma:
To contain soluble nickel salt, cobalt salt and manganese salt, or nickel salt and cobalt salt, or nickel salt and manganese salt, one of perhaps said three kinds of salt carry out precipitation reaction with the sodium hydroxide solution that is mixed with ammoniacal liquor, and the formation structural formula is Ni
xCo
yMn
z(OH)
2The granular precursor of (x+y+z=1,0≤x≤1,0≤y≤1,0≤z≤1), washing, drying obtains nickel, cobalt and/or manganese hydroxide presoma;
(2) adulterated al element:
To go up the resulting nickel of step, cobalt and/or manganese hydroxide presoma and nanometer aluminum compound mol ratio by Al/D=0.01~0.05, with the lithium salts mol ratio by Li/ (D+Al)=1.0~1.2; Mix; Make it to mix; Said D=Ni+Co+Mn or Ni+Co, Ni+Mn or Mn+Co, or Ni, Co, Mn any;
(3) high-temperature process:
The mixture of last step gained is carried out high-temperature process, and cooling is then pulverized, and sieves and promptly obtains the anode material for lithium-ion batteries of adulterated al element.
2. preparation method according to claim 1 is characterized in that: said nanometer aluminum compound is aluminium isopropoxide, aluminium oxide or aluminium hydroxide.
3. anode material for lithium-ion batteries, it is characterized in that: said anode material for lithium-ion batteries is to make according to each described preparation method in the claim 1 to 2.
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CN103178252A (en) * | 2013-03-18 | 2013-06-26 | 昆明理工大学 | Lithium ion battery anode material and preparation method thereof |
CN103606667A (en) * | 2013-11-26 | 2014-02-26 | 浙江南都电源动力股份有限公司 | Preparation method for manganese solid solution anode material of lithium ion battery material |
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