CN107959022A - A kind of solvent-thermal method prepares tertiary cathode material and preparation method thereof - Google Patents
A kind of solvent-thermal method prepares tertiary cathode material and preparation method thereof Download PDFInfo
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- 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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- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The invention discloses a kind of solvent-thermal method to prepare tertiary cathode material and preparation method thereof.This method is:Nickel cobalt manganese salt is dissolved in solvent, add surfactant and hydrolysis auxiliary agent, it is transferred to after being sufficiently stirred in reaction kettle, at a certain temperature after 2 24h of solvent thermal reaction, it is cooled to room temperature, nickel-cobalt-manganese ternary product is isolated using the method for suction filtration, after washed, dry, preroast in atmosphere obtains presoma;By presoma and lithium compound ground and mixed, roasting, is made tertiary cathode material;Ternary oxide presoma is compared with ternary precursor prepared by the usual precipitation method made from solvent-thermal method proposed by the invention, its particle has the advantages that size is small, it is regulatable with pattern to be evenly distributed, so that final obtained ternary material also has the characteristics that the important features such as granularity is small, particle diameter distribution is uniform, pattern is controllable, material shows excellent chemical property, its capacity and stability are superior to tertiary cathode material prepared by the precipitation method.
Description
Technical field
The present invention relates to ternary cathode material of lithium ion battery and its preparation, and in particular to a kind of solvent-thermal method prepares ternary
Positive electrode and preparation method thereof.
Background technology
Nickel-cobalt-manganese ternary anode material for lithium-ion batteries have it is of low cost, environmental-friendly, specific capacity is high, good cycle
With the important advantage such as security is good, extensively substitution cobalt acid lithium and LiFePO4 and as a kind of highly important lithium-ion electric
Pond positive electrode.
The method dominating process route of industrial production nickel-cobalt-manganternary ternary anode material is precipitation-mixed lithium-roasting method at present,
Nickel-cobalt-manganese ternary presoma is first generally made using the precipitation method, then with lithium salts (mainly lithium carbonate) mixed grinding, Ran Hou
Roasted under high temperature and ternary material is made.The common precipitation method prepare pattern and size Control of the ternary precursor there are presoma
The problem of more difficult, causing last obtained ternary material, there are granularity is larger, distribution of particles is uneven, pattern is irregular
The problems such as, it have impact on the performance of material property.To solve the problems, such as these, people have carried out substantial amounts of research in terms of preparation method
Work;Including adjustment precipitating reagent, solvent, addition auxiliary agent etc.;Such as:Chinese invention patent CN104810521A proposes a kind of oxidation
Coprecipitation, while it is aided with coating decoration, it is finally reached the purpose for improving material electrochemical performance;Chinese invention patent
CN106340642A is proposed, utilizes the tertiary cathode material for being catalyzed coprecipitation and preparing excellent performance.However, these effort are simultaneously
Not so that the pattern of material and distribution of particles problem are well solved;
For the precipitation method there are the problem of, there has been proposed sol-gal process in recent years.Such as:Chinese patent
In CN104916836A, using sol-gal process, it is aided with Supercritical Drying Technology, realizes the control of material granule size and size
System, prepares high-performance nickel-cobalt-manganternary ternary anode material.Although sol-gal process has the advantages of as described above, there is also original
The problems such as material is expensive, preparation process is complicated;Therefore, the new method of preparation high-performance tertiary cathode material is sought with particularly significant
Meaning.
The content of the invention
To solve the deficiencies in the prior art, the present invention proposes a kind of new solvent hot preparation nickel-cobalt-manganese ternary oxide
Method, this method are that nickel cobalt manganese presoma salt is dissolved in suitable solvent, by adjusting type of solvent and ratio and adding
Add suitable template, ternary oxide presoma of the synthesis with controllable appearance and size under the conditions of solvent heat.
The purpose of the present invention is realized at least through one of following technical solution.
A kind of solvent-thermal method prepares tertiary cathode material, and the positive electrode is layer structure, and chemical formula is:
LinNixCoyMnzO2, wherein 1.03≤n≤1.2,0.33≤x≤0.98,0.01≤y≤0.33,0.01≤z≤0.33, x+y+z
=1.
A kind of method that solvent-thermal method prepares tertiary cathode material, comprises the following steps:
(1) by a certain amount of nickel salt, cobalt salt and manganese salt addition deionized water and organic solvent mixed solution, (pure water is organic
Solvent) in, stirring and dissolving, labeled as solution A;Surfactant and hydrolysis auxiliary agent are dissolved in deionized water and are mixed with organic solvent
In solvent (pure water or organic solvent), stirring and dissolving, labeled as solution B;
(2) solution A is mixed with solution B, stirs 0.5h-20h, labeled as solution C,;Then solution C, which is transferred to, has
In the stainless steel cauldron of polytetrafluoroethyllining lining, 90 DEG C~200 DEG C insulation 6h~48h are risen to by room temperature;
(3) after after question response kettle is cooled to room temperature, product is filtered, washing, it is placed in 80-120 DEG C of dry 10- in drying box
24h, then prebake obtains nickel-cobalt-manganese ternary oxide precursor after firing at 200-600 DEG C;
(4) it is 1 according to the amount ratio of material by nickel-cobalt-manganese ternary oxide precursor and lithium compound:1.03~1.2, fill
After point mixed grinding, according to being roasted under certain heating schedule in air atmosphere.Be cooled to after room temperature i.e. be made particle size and
The tertiary cathode material Li of morphology controllablenNixCoyMnzO2。
In the above method, step (1) described nickel salt is one in nickel sulfate, nickel formate, nickel acetate, nickel chloride and nickel nitrate
More than kind;The cobalt salt is one or more of cobaltous sulfate, cobaltous formate, cobalt acetate, cobalt chloride and cobalt nitrate;The manganese salt is sulphur
One or more of sour manganese, formic acid manganese, manganese acetate, manganese chloride and manganese nitrate;The organic solvent is methanol, ethanol, isopropanol,
Polyethylene glycol, ethylene glycol, glycerine, propane diols, phenmethylol, benzyl carbinol, dimethylformamide, acetonitrile, dimethyl sulfoxide (DMSO), oleic acid
One or more of with oleyl amine;The surfactant is cetyl benzenesulfonic acid sodium, polyvinylpyrrolidone, cetyl three
In methyl bromide ammonium, lauryl sodium sulfate, hydroxyethyl cellulose, polyvinyl alcohol, enuatrol, sapn and tween it is a kind of with
On;The hydrolysis auxiliary agent is ammonium carbonate, ammonium hydrogen carbonate, oxalic acid, sodium carbonate, potassium carbonate, urea, ammonium formate, potassium hydroxide, hydrogen-oxygen
Change one or more of lithium, sodium hydroxide, sodium acetate, potassium acetate, lithium acetate, methenamine and ammonium fluoride.
In the above method, transition metal ions total soluble matters is 0.002~0.2mol/L in step (2) mixed solution C;It is described
Metal ion is Ni2+、Co2+And Mn2+;Surface-active additive amount is 1g/L~20g/L;Hydrolysis additive dosage is metal ion
0.5 times of the amount of total material~20 times;Deionized water accounts for the 0~100% of mixed solution C volume.
In the above method, in step (3), the roasting heating rate be 0.5~5 DEG C/min, calcination temperature is 200~
600 DEG C, roasting time is 4~10h.
In the above method, step (4) described lithium compound is lithium carbonate, lithium nitrate, lithium hydroxide, one kind of lithium acetate.
In the above method, in step (4), the roasting heating rate be 0.5~5 DEG C/min, calcination temperature is 700~
900 DEG C, when roasting time is 8~18 small.
Compared with prior art, advantage of the invention is that:
The present invention realizes the shape of nickel-cobalt-manganese ternary persursor material by the regulation and control to reaction condition during solvent heat
The Effective Regulation of looks and size, so as to significantly improve material electrochemical performance.Using this ternary oxide presoma as raw material
The tertiary cathode material of preparation is with the important advantage such as no ion mixing, particle uniform, morphology controllable, electrochemical performance.
The present invention provides a kind of important method, realizes the controllable of ternary material precursor (ternary oxide)
Standby, obtained ternary oxide material particle size is small, morphology controllable, particle diameter distribution are good;So that final obtained ternary material
Material shows excellent chemical property.
Brief description of the drawings
Fig. 1 is the tertiary cathode material (LiNi obtained by embodiment 10.5Co0.2Mn0.3O2) XRD diagram;
Embodiment
Make further specific detailed description, but embodiments of the present invention are not to the present invention with reference to specific embodiment
It is limited to this, for especially not dated technological parameter, can refer to routine techniques progress.
Embodiment 1
By nickel nitrate, cobalt nitrate, manganese sulfate in molar ratio 0.5:0.2:0.3 ratio is dissolved in a certain amount of deionized water and different
In propyl alcohol mixed solution, solution A is configured to.A certain amount of urea and polyvinylpyrrolidone are dissolved in deionized water and isopropanol
In mixed solution, solution B is configured to.After solution A is mixed with solution B, stir 0.5h, be configured to solution C, wherein, metal from
Sub- total concentration is 0.2mol/L, and polyvinylpyrrolidone additive amount is 1g/L, and hydrolysis additive dosage is metal ion total material
20 times of amount, deionized water accounts for the 10% of mixed solution C cumulative volume.Solution C is transferred to 50ml with polytetrafluoroethylene (PTFE)
Serve as a contrast in stainless steel cauldron, rise to 200 DEG C by room temperature, keep the temperature 10h.Products therefrom is filtered, is washed, after 80 DEG C of dry 10h, is put
In Muffle furnace, 200 DEG C of roasting 10h (roasting heating rate is 0.5 DEG C/min), obtain nickel-cobalt-manganese ternary oxygen under air atmosphere
Compound presoma.It is 1 that ternary oxide presoma and lithium carbonate are pressed amount of substance ratio:1.03 mixing, after being fully ground, air atmosphere
Lower 900 DEG C of roastings 8h (5 DEG C/min of roasting heating rate) is enclosed, is cooled to after room temperature and tertiary cathode material is made
LiNi0.5Co0.2Mn0.3O2.As seen from Figure 1, for the tertiary cathode material prepared without ion mixing, division peak is obvious, has
Good layer structure.
The main chemical property of material is shown in Table 1
Embodiment 2
By nickel acetate, cobalt acetate, manganese acetate in molar ratio 0.98:0.01:0.01 ratio is dissolved in a certain amount of deionized water
In triethanolamine mixed solution, solution A is configured to.A certain amount of methenamine and cetyl trimethylammonium bromide are dissolved in
In deionized water and triethanolamine mixed solution, solution B is configured to.After solution A is mixed with solution B, 20h is stirred, is configured to
Solution C, wherein, metal ion total concentration is 0.002mol/L, and cetyl trimethylammonium bromide additive amount is 15g/L, Wu Luo
Tropine additive amount is 0.5 times of the amount of metal ion total material, and deionized water accounts for the 80% of mixed solution C cumulative volume.By solution C
100ml is transferred to in polytetrafluoroethyllining lining stainless steel cauldron, 160 DEG C is risen to by room temperature, keeps the temperature 20h.Gained is produced
Thing is filtered, washing, after 80 DEG C of dry 15h, is placed in Muffle furnace, 600 DEG C of roasting 4h (roasting heating rates under air atmosphere
For 1 DEG C/min), obtain nickel-cobalt-manganese ternary oxide precursor.It is by amount of substance ratio with lithium acetate by ternary oxide presoma
1:1.05 mixing, after being fully ground, the lower 700 DEG C of roastings 18h of air atmosphere (0.5 DEG C/min of roasting heating rate), is cooled to room
Tertiary cathode material LiNi is made after temperature0.98Co0.01Mn0.01O2。
The main chemical property of material is shown in Table 1
Embodiment 3
By nickel chloride, cobalt chloride, manganese acetate in molar ratio 0.8:0.1:0.1 ratio is dissolved in deionized water solution, is matched somebody with somebody
It is set to solution A.Sodium acid carbonate and hydroxyethyl cellulose are dissolved in deionized water, are configured to solution B.Solution A and solution B are mixed
After conjunction, 5h is stirred, is configured to solution C, wherein, metal ion total concentration is 0.02mol/L, and hydroxyethyl cellulose additive amount is
10g/L, sodium acid carbonate additive amount are 5 times of the amount of metal ion total material.Solution C is transferred to 100ml has polytetrafluoroethyl-ne
In alkene inner liner stainless steel reaction kettle, 90 DEG C of insulation 2h are risen to by room temperature.By products therefrom it is filtered, washing, 80 DEG C of dry 24h
Afterwards, it is placed in Muffle furnace, 600 DEG C of roasting 4h (roasting heating rate is 5 DEG C/min), obtain nickel-cobalt-manganese ternary under air atmosphere
Oxide precursor.It is 1 that ternary oxide presoma and lithium acetate are pressed amount of substance ratio:1.1 mixing, after being fully ground, in sky
Atmosphere encloses lower 800 DEG C of roastings 18h (1 DEG C/min of roasting heating rate), is cooled to after room temperature and tertiary cathode material is made
LiNi0.8Co0.1Mn0.1O2。
The main chemical property of material is shown in Table 1
Embodiment 4
By nickel nitrate, cobalt nitrate, manganese nitrate in molar ratio 1:1:1 ratio is dissolved in ethanol solution, is configured to solution A.
Sodium acetate and polyvinylpyrrolidone are dissolved in ethanol solution, are configured to solution B.After solution A is mixed with solution B, stir
0.5h is mixed, is configured to solution C, wherein, metal ion total concentration is 0.05mol/L, and surface-active additive amount is 20g/L, acetic acid
Sodium additive amount is 5 times of the amount of metal ion total material.Solution C is transferred to 150ml has polytetrafluoroethyllining lining stainless steel
In reaction kettle, 180 DEG C of insulation 48h are risen to by room temperature.By products therefrom is filtered, washing, after 120 DEG C of dry 10h, Muffle is placed in
In stove, 200 DEG C of roasting 10h (roasting heating rate is 1 DEG C/min), obtain nickel-cobalt-manganese ternary oxide precursor under air atmosphere
Body.It is 1 that ternary oxide presoma and lithium hydroxide are pressed amount of substance ratio:1.2 mixing, after being fully ground mixing, air atmosphere
Lower 850 DEG C of roastings 8h (5 DEG C/min of roasting heating rate), is cooled to after room temperature and tertiary cathode material is made
LiNi0.33Co0.33Mn0.33O2。
The main chemical property of material is shown in Table 1
The main chemical property table of 1 each case study on implementation of table
The above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and is not to the present invention
Embodiment restriction.For those of ordinary skill in the field, can also make on the basis of the above description
Other various forms of changes or variation.There is no necessity and possibility to exhaust all the enbodiments.It is all the present invention
All any modification, equivalent and improvement made within spirit and principle etc., should be included in the protection of the claims in the present invention
Within the scope of.
Claims (7)
1. a kind of solvent-thermal method prepares tertiary cathode material, it is characterised in that the positive electrode is layer structure, chemical formula
For:LinNixCoyMnzO2, wherein 1.03≤n≤1.2,0.33≤x≤0.98,0.01≤y≤0.33,0.01≤z≤0.33,
x+y+z=1。
2. the method that solvent-thermal method described in claim 1 prepares tertiary cathode material, it is characterised in that comprise the following steps:
(1)Nickel salt, cobalt salt and manganese salt are added in solvent, the solvent is pure water, organic solvent is gone or ionized water with it is organic
Solvent mixed solution, stirring and dissolving, labeled as solution A;Surfactant and hydrolysis auxiliary agent are dissolved in solvent, the solvent is
Pure water or organic solvent or deionized water and organic solvent mixed solution, stirring and dissolving, labeled as solution B;
(2)Solution A is mixed with solution B, stirs 0.5h-20h, labeled as solution C,;Then solution C is transferred to poly- four
In the stainless steel cauldron of vinyl fluoride liner, 90 DEG C ~ 200 DEG C insulation 6h ~ 48h are risen to by room temperature;
(3)After after question response kettle is cooled to room temperature, product is filtered, washing, 80-120 DEG C of dry 10-24h in drying box is placed in,
Then prebake obtains nickel-cobalt-manganese ternary oxide precursor after firing at 200-600 DEG C;
(4)According to the amount ratio of material it is 1 by nickel-cobalt-manganese ternary oxide precursor and lithium compound:1.03 ~ 1.2, it is fully mixed
After closing grinding, roasted in air atmosphere, be cooled to the tertiary cathode material that particle size and morphology controllable are made after room temperature
Expect LinNixCoyMnzO2。
3. according to the method described in claim 2, it is characterized in that:Step(1)The nickel salt is nickel sulfate, nickel formate, acetic acid
One or more of nickel, nickel chloride and nickel nitrate;The cobalt salt is in cobaltous sulfate, cobaltous formate, cobalt acetate, cobalt chloride and cobalt nitrate
More than one;The manganese salt is one or more of manganese sulfate, formic acid manganese, manganese acetate, manganese chloride and manganese nitrate;It is described organic
Solvent is methanol, ethanol, isopropanol, polyethylene glycol, ethylene glycol, glycerine, propane diols, phenmethylol, benzyl carbinol, dimethyl formyl
One or more of amine, acetonitrile, dimethyl sulfoxide (DMSO), oleic acid and oleyl amine;The surfactant is cetyl benzenesulfonic acid sodium, gathers
Vinylpyrrolidone, cetyl trimethylammonium bromide, lauryl sodium sulfate, hydroxyethyl cellulose, polyvinyl alcohol, oleic acid
One or more of sodium, sapn and tween;The hydrolysis auxiliary agent is ammonium carbonate, ammonium hydrogen carbonate, oxalic acid, sodium carbonate, potassium carbonate, urine
In element, ammonium formate, potassium hydroxide, lithium hydroxide, sodium hydroxide, sodium acetate, potassium acetate, lithium acetate, methenamine and ammonium fluoride
More than one.
4. according to the method described in claim 2, it is characterized in that:Step(2)Transition metal ions total soluble matters in mixed solution C
For 0.002 ~ 0.2mol/L;The metal ion is Ni2+、Co2+And Mn2+;Surface-active additive amount is 1g/L ~ 20g/L;Hydrolysis
Additive dosage is 0.5 times ~ 20 times of the amount of metal ion total material;Deionized water accounts for the 0 ~ 100% of mixed solution C volume.
5. according to the method described in claim 2, it is characterized in that:Step(3)In, it is described roasting heating rate for 0.5 ~ 5 DEG C/
Min, calcination temperature are 200 ~ 600 DEG C, and roasting time is 4 ~ 10h.
6. according to the method described in claim 2, it is characterized in that:Step(4)The lithium compound for lithium carbonate, lithium nitrate,
One kind of lithium hydroxide, lithium acetate.
7. according to the method described in claim 2, it is characterized in that, step(4)In, it is described roasting heating rate for 0.5 ~ 5 DEG C/
Min, calcination temperature are 700 ~ 900 DEG C, when roasting time is 8 ~ 18 small.
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