CN108128814A - A kind of preparation method of ternary anode material precursor - Google Patents
A kind of preparation method of ternary anode material precursor Download PDFInfo
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- 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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Abstract
The invention discloses a kind of preparation methods of ternary anode material precursor, addition time, additive amount and the reaction condition of reactant during coprecipitation reaction are adjusted by specific aim, make the ternary anode material precursor granular size being prepared evenly, particle diameter distribution is narrower, cyclicity with its tertiary cathode material being prepared is more preferable, there is positive effect to the performance for improving lithium ion battery, and the preparation method is simple, reliable, of low cost, be suitble to ternary anode material precursor it is extensive, commercially produce.
Description
Technical field
Invention is related to anode material for lithium-ion batteries, more particularly to a kind of preparation method of ternary anode material precursor.
Background technology
The advantages that lithium ion battery is due to its high-energy density, security performance is preferable and cost is relatively low is most important at present
Electrochemical secondary cell.In lithium ion battery, due to unique lithium source that positive electrode is lithium ion battery, so, anode
The performance of material plays a key effect to the performance of lithium ion battery.In commercialization positive electrode LiCoO at present2、LiMn2O4、
LiFePO4、LiNi1-x-yCoxMnyO2（Tertiary cathode material）, due to, tertiary cathode material has relatively preferable comprehensive performance,
So in following 2-3, tertiary cathode material is likely to become the main positive electrode of motive-power battery.
At present, tertiary cathode material synthesis technology is：Ternary anode material precursor is first prepared by coprecipitation
（Ni1-x-yCoxMny(OH)2）；Ternary anode material precursor is mixed into lithium source again, tertiary cathode material is obtained after calcining.At this
In technique, Ni1-x-yCoxMny(OH)2Influence of the physical and chemical performance to the physical and chemical performance of tertiary cathode material it is very big.Especially, three
The uniformity of first positive electrode material precursor（Particle diameter distribution）It is affected to the cycle performance of tertiary cathode material, tertiary cathode material
The particle diameter distribution of material precursor is narrower, and the particle of obtained tertiary cathode material is more uniform, in charge and discharge process, each ternary
The de- lithium of positive electrode particle/embedding lithium degree more they tends to unanimously, so that the cyclicity of tertiary cathode material is with regard to more preferable.Therefore, it obtains
The particle diameter distribution of the ternary anode material precursor obtained is narrower（High uniformity）, be more conducive to promoted tertiary cathode material cycle
Performance.In order to obtain the narrower ternary anode material precursor of particle diameter distribution, at present generally according to grain size to tertiary cathode material
The method that presoma carries out secondary grading, but this method needs additional classifying equipoment and corresponding technique, causes production cost
Increase；In addition, before addition surfactant can also improve prepared tertiary cathode material during the coprecipitation reaction
The uniformity of body is driven, but the addition of surfactant also results in the increase of cost（Cost including surfactant and after
The cost of continuous wastewater treatment）.
Invention content
The ternary anode material precursor grain size point that it is an object of the invention to existing coprecipitation method is overcome to be prepared
A kind of the defects of cloth is wider, it is proposed that preparation method of ternary anode material precursor.This method is adjusted coprecipitated by specific aim
Addition time, additive amount and the reaction condition of reactant in the reaction process of shallow lake, so as to get ternary anode material precursor grain size
It is distributed narrower, the cyclicity with its tertiary cathode material being prepared is more preferable, has product to the performance for improving lithium ion battery
Pole acts on.
In order to achieve the above-mentioned object of the invention, the present invention provides a kind of preparation method of ternary anode material precursor, packets
Include following steps：
（1）The preparation of submicron particles：It is in inert gas shielding, pH value by transition metal salt solution and hydroxide solution
8-12, temperature carry out coprecipitation reaction 1-3h under conditions of being 25-60 DEG C, obtain the mixed solution containing submicron particles；
（2）The preparation of ternary anode material precursor：In step（1）Ammonium hydroxide is added in the mixed solution being prepared, is obtained anti-
Solution is answered, and transition metal salt solution and hydroxide solution are continuously added in reaction solution, in inert gas shielding, pH value
Carry out coprecipitation reaction 15-30h under conditions of being 30-80 DEG C for 10-12, temperature, it is filtered, wash and be dried to obtain ternary just
Pole material precursor.
A kind of preparation method of ternary anode material precursor of the present invention, using reaction condition to coprecipitation reaction product object
Change the influence of performance, first pass through temperature, pH value and the time of control coprecipitation reaction, generate dispersibility preferably submicron order
Grain, so as to reduce the intergranular generation being adhered with agglomeration；It recycles ammonium hydroxide that can promote the effect of coprecipitation reaction, passes through
Controlling reaction temperature, pH value and time using submicron particles as nucleating agent, steadily, quickly generate tertiary cathode material
Presoma, obtains that ternary anode material precursor grain shape is more regular, and evenly, particle diameter distribution is narrower for size；And this method
Simply, it is reliable, of low cost, be suitble to ternary anode material precursor it is extensive, commercially produce.
A kind of preparation method of above-mentioned ternary anode material precursor, wherein, coprecipitation reaction condition further includes in step 1
The ammonia environment of a concentration of 0 ~ 0.05mol/L；Ammonia concn is excessively high, and the nucleation rate of submicron particles is low, submicron particles
Quantity is few, also, the speed of growth of submicron particles is too fast, causes the in irregular shape of submicron particles.
A kind of preparation method of above-mentioned ternary anode material precursor, wherein, it is preferred that the co-precipitation described in step 1
The pH value of reaction is 11.0-11.5, and temperature is 55 DEG C；In the preferred scope, the submicron particles being prepared are dispersed
It is best.
A kind of preparation method of above-mentioned ternary anode material precursor, wherein, the inert gas packet described in step 1 and 2
It includes one or more in the inert gases such as nitrogen, helium or neon.
A kind of preparation method of above-mentioned ternary anode material precursor, wherein, the transition metal in step 1 and 2
Salt includes Ni salt, Mn salt and Co salt；Ni salt, Mn salt and the Co salt, which refers to ionize in aqueous solution, generates nickel ion, manganese
The compound of ion and cobalt ions；Preferably, the Ni salt includes one or more in nickel sulfate, nickel nitrate, nickel chloride；
The Mn salt includes one or more in manganese sulfate, manganese nitrate, manganese chloride；The Co salt include cobaltous sulfate, cobalt nitrate,
It is one or more in cobalt chloride.Most preferably, the Ni salt is nickel sulfate；The Mn salt is manganese sulfate；The Co
Salt includes cobaltous sulfate；By preferred, the submicron particles dispersibility being prepared is more preferable, the grain of ternary anode material precursor
Diameter distribution is narrower.
Wherein, the transition metal salt solution substance withdrawl syndrome is 1.5-2.5mol/L, and concentration is excessive（＞
2.5mol/L）, transition metal ions concentration is big, and transition metal salt easily crystallizes precipitation, be unfavorable for coprecipitation reaction generation and
Industrialized production；Concentration is too small（＜ 1.5mol/L）, low production efficiency, and wastewater flow rate is big；Preferably, the transition metal
Concentration of salt solution is 2.0mol/L.
A kind of preparation method of above-mentioned ternary anode material precursor, wherein, the hydroxide described in step 1 and 2 is
One or both of sodium hydroxide, potassium hydroxide；The wherein described hydroxide solution substance withdrawl syndrome is 2.0-
8.0mol/L, concentration are excessive（＞ 8.0mol/L）, solution easily crystallizes precipitation, is unfavorable for the generation and industrialization of coprecipitation reaction
Production；Concentration is too small（＜ 2.0mol/L）, low production efficiency, and wastewater flow rate is big.Preferably, the hydroxide solution is dense
It spends for 5.0mol/L.
A kind of preparation method of above-mentioned ternary anode material precursor, wherein, the ammonia concn in step 2 in reaction solution
For 0.1 ~ 1.0 mol/L；For ammonium hydroxide as complexing agent, concentration influences the formation speed of ternary anode material precursor, and ammonium hydroxide is used
Measure excessive, ternary anode material precursor formation speed is fast, causes grain shape irregular, and grain size difference is big, and particle diameter distribution is wide；
And ammonia volume is too small, ternary anode material precursor particle diameter distribution is narrow, but formation speed is slow, and industrial production efficiency is low；It is preferred that
, the ammonia concn in the reaction solution is 0.3 mol/L.
A kind of preparation method of above-mentioned ternary anode material precursor, wherein, it is preferred that the co-precipitation described in step 2
The pH value of reaction is 11, and temperature is 50 DEG C；In the preferred scope, the ternary anode material precursor particle being prepared is more equal
Even, particle diameter distribution is narrower.
Compared with prior art, beneficial effects of the present invention：
1st, the preparation method of ternary anode material precursor of the present invention, the ternary anode material precursor granular size being prepared
Evenly, particle diameter distribution is narrower, and the cyclicity with its tertiary cathode material being prepared is more preferable, to improving lithium ion battery
Performance has positive effect.
2nd, the preparation method of ternary anode material precursor of the present invention is that grain size is directly prepared by coprecipitation reaction
Narrower ternary anode material precursor particle is distributed, does not both need to carry out secondary grading processing, also without addition surface-active
Production cost has been saved in agent, simplifies processing step.
3rd, preparation method of the present invention is simple, reliable, of low cost, is suitble to extensive, the quotient of ternary anode material precursor
Industry metaplasia is produced.
Description of the drawings：
Fig. 1 is the process flow chart of the preparation method of ternary anode material precursor of the present invention.
Fig. 2 is the SEM figures of ternary anode material precursor prepared by embodiment 1.
Fig. 3 is the SEM figures of ternary anode material precursor prepared by comparative example.
Specific embodiment
With reference to comparative example and specific embodiment, the present invention is described in further detail.But this should not be understood
Range for the above-mentioned theme of the present invention is only limitted to following embodiment, all to belong to this based on the technology that the content of present invention is realized
The range of invention.
Embodiment 1
1st, the preparation of submicron particles：By the MSO of 2.0mol/L4（M=Ni, Co, Mn, wherein Ni ︰ Co ︰ Mn molar ratios are
0.8 ︰, 0.1 ︰ 0.1）Reaction vessel is added dropwise with the speed of 1ml/min respectively in the NaOH solution of solution and 5.0mol/L, meanwhile,
Nitrogen is passed through, coprecipitation reaction 1h is carried out under conditions of pH value is 11.0, temperature is 55 DEG C, is obtained containing submicron particles
Mixed solution；
2nd, the preparation of ternary anode material precursor：In step（1）Ammonium hydroxide is added in the mixed solution being prepared, is reacted
Solution, and the ammonia concn of reaction solution is controlled in 0.3mol/L, continuously add the MSO of 2.0mol/L4（M=Ni, Co, Mn,
Wherein Ni ︰ Co ︰ Mn molar ratios are 0.8 ︰, 0.1 ︰ 0.1）The NaOH solution of solution and 5.0mol/L continues to be passed through nitrogen, in pH value
Coprecipitation reaction 25h is carried out under conditions of being 50 DEG C for 11.0, temperature, it is filtered, wash and be dried to obtain after the completion of reaction
Ni0.8Co0.1Mn0.1(OH)2Particle, i.e. ternary anode material precursor（Its SEM figure is Fig. 2）.
After testing, the Ni being prepared0.8Co0.1Mn0.1 (OH)2Particle uniformity is high, D10It is 7.5 microns, D50It is 10.1
Micron, D90It is 12.3 microns.
Embodiment 2
1st, the preparation of submicron particles：By the MCl of 2.5mol/L2（M=Ni, Co, Mn, wherein Ni ︰ Co ︰ Mn molar ratios are
0.7 ︰, 0.1 ︰ 0.2）Reaction vessel is added dropwise with the speed of 2ml/min respectively in the KOH solution of solution and 2.0mol/L, meanwhile,
Ammonium hydroxide is added in, and it is 0.02mol/L to control ammonia concn in solution, nitrogen is passed through, in the item that pH value is 12.0, temperature is 25 DEG C
Coprecipitation reaction 1h is carried out under part, obtains the mixed solution containing submicron particles；
2nd, the preparation of ternary anode material precursor：In step（1）Ammonium hydroxide is added in the mixed solution being prepared, is reacted
Solution, and ammonia concn in reaction solution is controlled in 0.1mol/L, continuously add the MCl of 2.0mol/L2（M=Ni, Co, Mn,
Wherein Ni ︰ Co ︰ Mn molar ratios are 0.7 ︰, 0.1 ︰ 0.2）The KOH solution of solution and 2.0mol/L, continues to be passed through nitrogen, is in pH value
8.0th, temperature is carries out coprecipitation reaction 30h under conditions of 40 DEG C, filtered, wash and be dried to obtain after the completion of reaction
Ni0.7Co0.1Mn0.2(OH)2Particle, i.e. ternary anode material precursor.
After testing, the Ni being prepared0.7Co0.1Mn0.2(OH)2Particle uniformity is high, D10It is 6.8 microns, D50It is micro- for 12.4
Rice, D90It is 15.6 microns.
Embodiment 3
1st, the preparation of submicron particles：By the M (NO of 1.5mol/L3)2（M=Ni, Co, Mn, wherein Ni ︰ Co ︰ Mn molar ratios are
0.6 ︰, 0.2 ︰ 0.2）Reaction vessel is added dropwise with the speed of 0.5.ml/min respectively in the KOH solution of solution and 8.0mol/L, leads to
Enter nitrogen, coprecipitation reaction 3h is carried out under conditions of pH value is 8.0, temperature is 45 DEG C, is obtained containing submicron particles
Mixed solution；
2nd, the preparation of ternary anode material precursor：In step（1）Ammonium hydroxide is added in the mixed solution being prepared, is reacted
Solution, and ammonia concn in reaction solution is controlled in 0.2mol/L, continuously add the M (NO of 1.5mol/L3)2（M= Ni、Co、
Mn, wherein Ni ︰ Co ︰ Mn molar ratios are 0.6 ︰, 0.2 ︰ 0.2）The KOH solution of solution and 8.0mol/L continues to be passed through nitrogen, in pH
Be worth for 12.0, temperature be 80 DEG C under conditions of carry out coprecipitation reaction 15h, it is filtered, wash and be dried to obtain after the completion of reaction
Ni0.6Co0.2Mn0.2(OH)2Particle, i.e. ternary anode material precursor.
After testing, the Ni being prepared0.6Co0.2Mn0.2 (OH)2Particle uniformity is high, D10It is 7.7 microns, D50It is 12.3
Micron, D90It is 15.2 microns.
Embodiment 4
1st, the preparation of submicron particles：By the MSO of 2.0mol/L4（M=Ni, Co, Mn, wherein Ni ︰ Co ︰ Mn molar ratios are
0.6 ︰, 0.2 ︰ 0.2）Reaction vessel is added dropwise with the speed of 1ml/min respectively in the NaOH solution of solution and 5.0mol/L, meanwhile,
Ammonium hydroxide is added in, and it is 0.05mol/L to control ammonia concn in solution, nitrogen is passed through, in the item that pH value is 11.5, temperature is 50 DEG C
Coprecipitation reaction 2h is carried out under part, obtains the mixed solution containing submicron particles；
2nd, the preparation of ternary anode material precursor：In step（1）Ammonium hydroxide is added in the mixed solution being prepared, is reacted
Solution, and ammonia concn in reaction solution is controlled in 1.0mol/L, continuously add the MSO of 2.0mol/L4（M=Ni, Co, Mn,
Wherein Ni ︰ Co ︰ Mn molar ratios are 0.6 ︰, 0.2 ︰ 0.2）The NaOH solution of solution and 5.0mol/L continues to be passed through nitrogen, in pH value
Coprecipitation reaction 25h is carried out under conditions of being 50 DEG C for 11.0, temperature, it is filtered, wash and be dried to obtain after the completion of reaction
Ni0.6Co0.2Mn0.2(OH)2Particle, i.e. ternary anode material precursor.
After testing, the Ni being prepared0.6Co0.2Mn0.2 (OH)2Particle uniformity is high, D10It is 6.9 microns, D50It is 10.1
Micron, D90It is 12.5 microns.
Comparative example
By the MSO of 2.0mol/L4（M=Ni, Co, Mn, wherein Ni ︰ Co ︰ Mn molar ratios are 0.8 ︰, 0.1 ︰ 0.1）Solution with
Reaction vessel is added dropwise with the speed of 1ml/min respectively in the NaOH solution of 5.0mol/L, meanwhile, ammonium hydroxide is added in, is reacted
Solution, and ammonia concn control in reaction solution in 0.3mol/L, is passed through nitrogen, pH value is 11.0, temperature is 50 DEG C
Under the conditions of carry out coprecipitation reaction 26 hours, it is after reaction, filtered, wash and be dried to obtain Ni0.8Co0.1Mn0.1(OH)2
Particle, i.e. ternary anode material precursor（Its SEM figure is Fig. 3）.
After testing, the Ni being prepared0.8Co0.1Mn0.1(OH)2Particle is uneven, D10It is 4.4 microns, D50It is micro- for 11.6
Rice, D90It is 19.8 microns.
Claims (10)
1. a kind of preparation method of ternary anode material precursor, which is characterized in that include the following steps：
（1）The preparation of submicron particles：It is in inert gas shielding, pH value by transition metal salt solution and hydroxide solution
8-12, temperature carry out coprecipitation reaction 1-3h under conditions of being 25-60 DEG C, obtain the mixed solution containing submicron particles；
（2）The preparation of ternary anode material precursor：In step（1）Ammonium hydroxide is added in the mixed solution being prepared, is obtained anti-
Solution is answered, and transition metal salt solution and hydroxide solution are continuously added in reaction solution, in inert gas shielding, pH value
Carry out coprecipitation reaction 15-30h under conditions of being 30-80 DEG C for 10-12, temperature, it is filtered, wash and be dried to obtain ternary just
Pole material precursor.
2. preparation method according to claim 1, which is characterized in that step（1）Middle coprecipitation reaction condition further includes dense
Spend the ammonia environment for 0 ~ 0.05 mol/L.
3. preparation method according to claim 1, which is characterized in that step（1）Described in coprecipitation reaction pH value
For 11.0-11.5, temperature is 55 DEG C.
4. preparation method according to claim 1, which is characterized in that step（1）With（2）Described in inert gas include
It is one or more in the inert gases such as nitrogen, helium or neon.
5. preparation method according to claim 1, which is characterized in that step（1）With（2）In the transition metal salt
Including Ni salt, Mn salt and Co salt.
6. preparation method according to claim 5, which is characterized in that the Ni salt includes nickel sulfate, nickel nitrate, chlorination
It is one or more in nickel；The Mn salt includes one or more in manganese sulfate, manganese nitrate, manganese chloride；The Co salt
Including one or more in cobaltous sulfate, cobalt nitrate, cobalt chloride.
7. preparation method according to claim 1, which is characterized in that step（1）With（2）Described in hydroxide be hydrogen
One or both of sodium oxide molybdena, potassium hydroxide.
8. preparation method according to claim 1, which is characterized in that step（2）Ammonia concn in middle reaction solution is
0.1~1.0 mol/L。
9. preparation method according to claim 8, which is characterized in that step（2）Ammonia concn in middle reaction solution is
0.3mol/L。
10. preparation method according to claim 1, which is characterized in that step（2）Described in coprecipitation reaction pH value
It is 11, temperature is 50 DEG C.
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| CN111509205A (en) * | 2020-04-21 | 2020-08-07 | 江门市科恒实业股份有限公司 | Ternary cathode material for zirconium-coated lithium ion battery and preparation method thereof |
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