CN103227322A - Quaternary lithium-ion battery positive electrode material and preparation method thereof - Google Patents
Quaternary lithium-ion battery positive electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a quaternary lithium-ion battery positive electrode material and a preparation method thereof. A molecular formula of the quaternary lithium-ion battery positive electrode material is LiNi0.8Co0.15Al0.03Mn0.02O2, a 0.2 C discharge capacity at a room temperature of 180-185mAh/g; and weight ratio energy is 650-661 Wh/Kg. The LiNi0.8Co0.15Al0.03Mn0.02O2 prepared by the method has a uniform sphere structure, and at the same time, due to the effect of a template, the prepared quaternary lithium-ion battery positive electrode material is beneficial to store electrolyte and overcome capacity loss caused by incomplete reaction of materials at core part. The quaternary lithium-ion battery positive electrode material greatly increases storage energy of the material, can prepare lithium ion power battery with light weight and high capacity, and can be widely applied in situations of electrical vehicles, electric bicycles, electric tools, etc.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries.
Background technology
Lithium ion battery has the specific energy height, and is in light weight, and characteristics such as safety and environmental protection, stable performance have been widely used in numerous fields that need energy carrier such as mobile phone and digital electrical apparatus, electric automobile, electric tool.Commercial in the market lithium ion battery can be divided into ferric phosphate lithium cell, cobalt acid lithium battery, ternary material battery etc. according to the difference of positive electrode.Wherein, the ferric phosphate lithium cell specific energy is lower, can only reach 100～130Wh/Kg, but fail safe is best.Cobalt acid lithium and ternary material battery can reach the high-energy-density, particularly cobalt acid lithium battery near 200Wh/Kg, and volumetric specific energy has reached 550Wh/L at present.The shortcoming of above battery system is: cobalt acid lithium and tertiary cathode material all contain more expensive cobalt element, cause to hold at high price.In addition, from national development strategy, the specific energy about 200Wh/Kg still can not meet the demands, and the lithium-ion battery system specific energy of used for electric vehicle should could satisfy user's requirement at 250Wh/Kg at least.
From the development trend of lithium ion battery, should be under the prerequisite that reduces cost, increase substantially energy density.At present, the room for improvement of negative material is little, can only lean on the energy density of the improvement raising battery of positive electrode.The improvement direction of positive electrode is to improve specific capacity and discharge voltage.At present, the development trend of tertiary cathode material system is the nickel content ratio that improves wherein.Nickel content is high more, and specific energy is big more.LiNi
0.33Co
0.33Mn
0.33O
2Generally have only the specific capacity about 145mAh/g, and LiNi
0.5Co
0.2Mn
0.3O
2Can reach about 160mAh/g LiNi
0.8Co
0.15Al
0.05O
2Or LiNi
0.8Co
0.15Mn
0.05O
2Can reach more than the 180mAh/g.Adopt LiNi
0.8Co
0.15Al
0.05O
2Making battery can make the specific energy of battery reach more than the 250Wh/Kg.
Above material system is from research doping lithium nickelate (LiNiO
2) material begins.According to people such as Chebiam (Structuralinstability of delithiated Li
1-xNi
L-yCo
yO
2Cathodes.Journal of the Electrochemical Society, 2001,148:A49～53) research is at x＜0.25 o'clock, Li
xNi
0.85Co
0.15O
2(H2 and H3) is in when taking off the lithium state entirely, only has a kind of cube of phase (H3).This behavior and LiCoO
2(x Oxygen loss in＜0.45 o'clock) the same, this just causes actual capacity low.In order further to improve LiNi
1-yCo
yO
2The chemical property of positive electrode and thermal stability, researchers replace the nickel cobalt with other cationic moiety.Al replaces the structural stability that Ni/Co also can improve material to a certain extent, improves the charging cycle stability of material.Along with the development of technology, LiNi
L-x-yCo
xAl
yO
2Positive electrode has also obtained great concern, LiNi
L-x-yCo
xAl
yO
2Material is considered to have the anode material for lithium-ion batteries of new generation of application prospect.
For a long time, there is bigger technical barrier in the preparation of the positive electrode of high nickel content.For example, the sintering difficulty, there are defectives such as mixing easily in metal cation, and there are problems such as oxidation is incomplete easily in nickel, particularly appraises at the current rate to have the Jahn-Teller effect when insufficient and make cycle performance relatively poor.
Traditional LiNi
L-x-yCo
xAl
yO
2Material synthesis method has high temperature solid-state method, sol-gel process, coprecipitation etc.High-temperature solid phase reaction method is that the solid material mixture is directly carried out high temperature sintering with solid-state form.Traditional high temperature solid-state method synthesis technique is simple, and equipment requirements is low, and synthesis condition is controlled easily, and environmental protection is the prefered method of large-scale production.People have carried out extensive studies to high temperature solid-state method, mainly concentrate on reaction raw materials, raw material proportioning, reaction temperature and reaction atmosphere etc. to the structure of lithium-nickel-cobalt-oxygen thing and the influence of chemical property.From reducing reaction temperature and stable Ni
3+Angle set out, proper with the oxide or the hydroxide of lithium, nickel, cobalt as raw material.Yet because the particle of raw material is big, nickel cobalt ions diffusion rate is slow, and the synthetic material of conventional solid-state method often exists reaction not exclusively, problems such as crystal perfection difference, even the local LiNiO of generation appears
2And LiCoO
2The phenomenon of mixture causes the chemical property of material poor.Coprecipitation can accurately be controlled each components contents, makes each element realize other the even mixing of molecule/atomic level level, and the synthesis temperature that helps reducing material (can reduce Ni
2+Generation), improve the chemical property and the physical property of material.Yet, adopting general coprecipitation, mostly synthetic material is that sheet or polygonal etc. are irregularly shaped, has serious agglomeration.Tap density, physical properties such as uniform particles degree are poor, are difficult to satisfy the requirement of the high-bulk-density and the high-volume and capacity ratio of positive electrode.Sol-gel process is with organic substance and cation generation complexing with complexing function, under liquid phase state, make the mixing on each component realization molecule or the atomic level, by processes such as hydrolysis, condensation, nucleation, growths, in solution, form stable vitreosol system, colloidal sol forms the gel with three-dimensional space network structure through slowly polymerization.Gel synthesizes the material of micron and even Nano grade through super-dry, sintering curing.The synthetic powder body material of sol-gel process has composition evenly (can be realized evenly mixing on atom or the molecular level), and powder granule is tiny, can reach micron even Nano grade, and particle size distribution range is narrow, and technological process is simple, easy control of reaction conditions.But the organic reagent that sol-gel process consumes is many, and cost and environment are had very big unfavorable factor.In dry run, because the viscosity of colloidal sol is bigger, arid cycle is longer relatively.Owing to have more organic substance macromolecule, have very big volumetric expansion effect in the gelinite.In removing organic process, the shrinkage degree of gelinite is big.The sintering character of powder body material is poor, and synthesis condition is also than solid phase method harshness.Above-mentioned unfavorable factor causes the productivity ratio of material low, the cost height.At present, the technology of sol-gel process synthesis of anode material of lithium-ion battery does not also reach industrial production requirement.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of quaternary anode material for lithium-ion batteries is provided.
Second purpose of the present invention provides a kind of preparation method of quaternary anode material for lithium-ion batteries.
Technical scheme of the present invention is summarized as follows:
A kind of quaternary anode material for lithium-ion batteries, the molecular formula of described quaternary anode material for lithium-ion batteries is LiNi
0.8Co
0.15Al
0.03Mn
0.02O
2, room temperature 0.2C discharge capacity is 180-185mAh/g, gravimetric specific energy is 650-661Wh/Kg.
The preparation method of above-mentioned a kind of quaternary anode material for lithium-ion batteries comprises the steps:
(1) the spherical masterplate emulsion of preparation takes by weighing by weight percentage: mineral oil 5-8%, and non-ionic surface active agent 10%-40%, defoamer 0.1%-1%, anticorrisive agent 0.01%-0.5%, surplus is a distilled water; Mix and stirred 1-5 hour, obtain milky white liquid;
(2) be the 80:15:3:2 ratio in molar ratio, nickel salt, cobalt salt, aluminium salt and manganese salt be dissolved in the water that the concentration of making nickel salt, cobalt salt, aluminium salt and manganese salt sum is the solution of 0.5～2mol/L; Described nickel salt is preferably nickelous sulfate or nickel nitrate, and described cobalt salt is preferably cobaltous sulfate or cobalt nitrate, and described aluminium salt is preferably aluminum sulfate or aluminum nitrate, and described manganese salt is preferably manganese sulfate or manganese nitrate;
(3) by weight be 1:(10～20) ratio, the liquid that step (1) is obtained joins in the solution of step (2) acquisition, stirs 1～3 hour;
(4) under agitation, with 15～30 hours, adding concentration in the liquid that step (3) obtains was lithium hydroxide aqueous solution or the sodium hydrate aqueous solution of 1～8mol/L, and making the pH value is 10～13, makes (the Ni of generation
0.8Co
0.15Al
0.03Mn
0.02) (OH)
2Even laminating is deposited to spherical reticle surface, leaves standstill to wear out in 24～48 hours, forms spherical presoma;
(5) be that 9～11 ammoniacal liquor fully washs with presoma pH, remove lithium ion or sodium ion, and sulfate ion or nitrate ion, in the 1mol presoma: the ratio of 100～1000 ml distilled waters, being scattered in the distilled water, is the ratio of 100:80 in the mol ratio with nickel salt, adds lithium hydroxide, dissolving is even, and spray drying is made the presoma that lithium hydroxide evenly coats;
(6) presoma that evenly coats of the lithium hydroxide that step (5) is obtained, 700～900 ℃ of calcining at constant temperature 12～48 hours, the content of constant temperature stage oxygen was 40%-65%; With cooling rate is that 3～10 ℃/minute speed is cooled to room temperature, pulverizes through airslide disintegrating mill, through grader classification, the quaternary anode material for lithium-ion batteries LiNi that obtains having spherical morphology
0.8Co
0.15Al
0.03Mn
0.02O
2
Preferred No. 10 machine oil of mineral oil or No. 20 machine oil.
Non-ionic surface active agent is preferred: APES (APEO), AEO (AEO) or polyoxyethylene carboxylate (AE).
The preferred dimethicone of defoamer.
Preferred sorbierite of anticorrisive agent or benzoic acid.
The invention has the beneficial effects as follows:
The LiNi that the present invention makes
0.8Co
0.15Al
0.03Mn
0.02O
2Have the uniform spherical structure,, make the quaternary anode material for lithium-ion batteries of preparation, help storing electrolyte, and overcome the capacitance loss that the reaction of core active material not exclusively causes simultaneously owing to the effect of masterplate.Confirm according to result of the test, the quaternary anode material for lithium-ion batteries that adopts method of the present invention to obtain, its room temperature 0.2C discharge capacity can reach 180-185mAh/g, and gravimetric specific energy reaches 650-661Wh/Kg, has improved the energy storage energy of material greatly.The quaternary anode material for lithium-ion batteries of method preparation of the present invention can be made lithium-ion-power cell in light weight, that capacity is high, is widely used in occasions such as electric automobile, electric bicycle, electric tool, improves the overall performance of system greatly.
Embodiment
The principle of foundation is: stable element Al in ternary material substitutes with Al and Mn, utilizes composite mixed cooperative effect, realizes the stable of material lattice system better, makes material reduce distortion of lattice deviating from lithium ion.
The following examples are in order to enable those skilled in the art to understand better the present invention, but the present invention are not imposed any restrictions.
Embodiment 1
A kind of preparation method of quaternary anode material for lithium-ion batteries comprises the steps:
(1) the spherical masterplate emulsion of preparation takes by weighing by weight percentage: No. 10 machine oil 5%, and APES (APEO) 10%, dimethicone 0.1%, sorbierite 0.01%, surplus is a distilled water; Mix and stirred 1 hour, obtain milky white liquid;
(2) be the 80:15:3:2 ratio in molar ratio, nickelous sulfate, cobaltous sulfate, aluminum sulfate and manganese sulfate be dissolved in the water that the concentration of making nickelous sulfate, cobaltous sulfate, aluminum sulfate and manganese sulfate sum is the solution of 0.5mol/L;
(3) by weight being the ratio of 1:10, the liquid that step (1) is obtained joins in the solution of step (2) acquisition, stirs 1 hour;
(4) under agitation, with 15 hours, adding concentration in the liquid that step (3) obtains was the lithium hydroxide aqueous solution of 1mol/L, and making the pH value is 10, makes (the Ni of generation
0.8Co
0.15Al
0.03Mn
0.02) (OH)
2Even laminating is deposited to spherical reticle surface, leaves standstill to wear out in 48 hours, forms spherical presoma;
(5) be that 9 ammoniacal liquor fully washs with presoma pH, remove lithium ion and sulfate ion, in the 1mol presoma: the ratio of 100 ml distilled waters, be scattered in the distilled water, in the mol ratio with nickelous sulfate is the ratio of 100:80, add lithium hydroxide, dissolving is even, and spray drying is made the presoma that lithium hydroxide evenly coats;
(6) presoma that evenly coats of the lithium hydroxide that step (5) is obtained, 700 ℃ of calcining at constant temperature 48 hours, the content of constant temperature stage oxygen was 40%; With cooling rate is that 10 ℃/minute speed is cooled to room temperature, pulverizes through airslide disintegrating mill, through grader classification, the quaternary anode material for lithium-ion batteries LiNi that obtains having spherical morphology
0.8Co
0.15Al
0.03Mn
0.02O
2Room temperature 0.2C discharge capacity can reach 183mAh/g, and gravimetric specific energy reaches 659Wh/Kg.
Embodiment 2
A kind of preparation method of quaternary anode material for lithium-ion batteries comprises the steps:
(1) the spherical masterplate emulsion of preparation takes by weighing by weight percentage: No. 20 machine oil 6%, and AEO (AEO) 20%, dimethicone 0.5%, sorbierite 0.05%, surplus is a distilled water; Mix and stirred 2 hours, obtain milky white liquid;
(2) be the 80:15:3:2 ratio in molar ratio, nickel nitrate, cobalt nitrate, aluminum nitrate and manganese nitrate be dissolved in the water that the concentration of making nickel nitrate, cobalt nitrate, aluminum nitrate and manganese nitrate sum is the solution of 1mol/L;
(3) by weight being the ratio of 1:12, the liquid that step (1) is obtained joins in the solution of step (2) acquisition, stirs 2 hours;
(4) under agitation, with 20 hours, adding concentration in the liquid that step (3) obtains was the lithium hydroxide aqueous solution of 5mol/L, and making the pH value is 11, makes (the Ni of generation
0.8Co
0.15Al
0.03Mn
0.02) (OH)
2Even laminating is deposited to spherical reticle surface, leaves standstill to wear out in 36 hours, forms spherical presoma;
(5) be that 10 ammoniacal liquor fully washs with presoma pH, remove lithium ion and nitrate ion, in the 1mol presoma: the ratio of 500 ml distilled waters, be scattered in the distilled water, in the mol ratio with nickel nitrate is the ratio of 100:80, add lithium hydroxide, dissolving is even, and spray drying is made the presoma that lithium hydroxide evenly coats;
(6) presoma that evenly coats of the lithium hydroxide that step (5) is obtained, 800 ℃ of calcining at constant temperature 36 hours, the content of constant temperature stage oxygen was 45%; With cooling rate is that 7 ℃/minute speed is cooled to room temperature, pulverizes through airslide disintegrating mill, through grader classification, the quaternary anode material for lithium-ion batteries LiNi that obtains having spherical morphology
0.8Co
0.15Al
0.03Mn
0.02O
2Room temperature 0.2C discharge capacity can reach 185mAh/g, and gravimetric specific energy reaches 661Wh/Kg.
Embodiment 3
A kind of preparation method of quaternary anode material for lithium-ion batteries comprises the steps:
(1) the spherical masterplate emulsion of preparation takes by weighing by weight percentage: No. 10 machine oil 7%, and polyoxyethylene carboxylate (AE) 30%, dimethicone 0.8%, benzoic acid 0.1%, surplus is a distilled water; Mix and stirred 3 hours, obtain milky white liquid;
(2) be the 80:15:3:2 ratio in molar ratio, nickel nitrate, cobalt nitrate, aluminum nitrate and manganese nitrate be dissolved in the water that the concentration of making nickel nitrate, cobalt nitrate, aluminum nitrate and manganese nitrate sum is the solution of 1.5mol/L;
(3) by weight being the ratio of 1:15, the liquid that step (1) is obtained joins in the solution of step (2) acquisition, stirs 2 hours;
(4) under agitation, with 25 hours, adding concentration in the liquid that step (3) obtains was the sodium hydrate aqueous solution of 6mol/L, and making the pH value is 12, makes (the Ni of generation
0.8Co
0.15Al
0.03Mn
0.02) (OH)
2Even laminating is deposited to spherical reticle surface, leaves standstill to wear out in 30 hours, forms spherical presoma;
(5) be that 10 ammoniacal liquor fully washs with presoma pH, remove sodium ion and nitrate ion, in the 1mol presoma: the ratio of 800 ml distilled waters, be scattered in the distilled water, in the mol ratio with nickel nitrate is the ratio of 100:80, add lithium hydroxide, dissolving is even, and spray drying is made the presoma that lithium hydroxide evenly coats;
(6) presoma that evenly coats of the lithium hydroxide that step (5) is obtained, 850 ℃ of calcining at constant temperature 24 hours, the content of constant temperature stage oxygen was 55%; With cooling rate is that 6 ℃/minute speed is cooled to room temperature, pulverizes through airslide disintegrating mill, through grader classification, the quaternary anode material for lithium-ion batteries LiNi that obtains having spherical morphology
0.8Co
0.15Al
0.03Mn
0.02O
2Room temperature 0.2C discharge capacity can reach 183mAh/g, and gravimetric specific energy reaches 654Wh/Kg.
Embodiment 4
A kind of preparation method of quaternary anode material for lithium-ion batteries comprises the steps:
(1) the spherical masterplate emulsion of preparation takes by weighing by weight percentage: No. 20 machine oil 8%, and polyoxyethylene carboxylate (AE) 40%, dimethicone 1%, benzoic acid 0.5%, surplus is a distilled water; Mix and stirred 5 hours, obtain milky white liquid;
(2) be the 80:15:3:2 ratio in molar ratio, nickelous sulfate, cobaltous sulfate, aluminum sulfate and manganese sulfate be dissolved in the water that the concentration of making nickelous sulfate, cobaltous sulfate, aluminum sulfate and manganese sulfate sum is the solution of 2mol/L;
(3) by weight being the ratio of 1:20, the liquid that step (1) is obtained joins in the solution of step (2) acquisition, stirs 3 hours;
(4) under agitation, with 30 hours, adding concentration in the liquid that step (3) obtains was the sodium hydrate aqueous solution of 8mol/L, and making the pH value is 13, makes (the Ni of generation
0.8Co
0.15Al
0.03Mn
0.02) (OH)
2Even laminating is deposited to spherical reticle surface, leaves standstill to wear out in 24 hours, forms spherical presoma;
(5) be that 11 ammoniacal liquor fully washs with presoma pH, remove sodium ion and sulfate ion, in the 1mol presoma: the ratio of 1000 ml distilled waters, be scattered in the distilled water, in the mol ratio with nickelous sulfate is the ratio of 100:80, add lithium hydroxide, dissolving is even, and spray drying is made the presoma that lithium hydroxide evenly coats;
(6) presoma that evenly coats of the lithium hydroxide that step (5) is obtained, 900 ℃ of calcining at constant temperature 12 hours, the content of constant temperature stage oxygen was 65%; With cooling rate is that 3 ℃/minute speed is cooled to room temperature, pulverizes through airslide disintegrating mill, through grader classification, the quaternary anode material for lithium-ion batteries LiNi that obtains having spherical morphology
0.8Co
0.15Al
0.03Mn
0.02O
2Room temperature 0.2C discharge capacity can reach 180mAh/g, and gravimetric specific energy reaches 650Wh/Kg.
Claims (6)
1. quaternary anode material for lithium-ion batteries, the molecular formula that it is characterized in that described quaternary anode material for lithium-ion batteries is LiNi
0.8Co
0.15Al
0.03Mn
0.02O
2, room temperature 0.2C discharge capacity is 180-185mAh/g, gravimetric specific energy is 650-661Wh/Kg.
2. the preparation method of a kind of quaternary anode material for lithium-ion batteries of claim 1 is characterized in that comprising the steps:
(1) the spherical masterplate emulsion of preparation takes by weighing by weight percentage: mineral oil 5-8%, and non-ionic surface active agent 10%-40%, defoamer 0.1%-1%, anticorrisive agent 0.01%-0.5%, surplus is a distilled water; Mix and stirred 1-5 hour, obtain milky white liquid;
(2) be the 80:15:3:2 ratio in molar ratio, nickel salt, cobalt salt, aluminium salt and manganese salt be dissolved in the water that the concentration of making nickel salt, cobalt salt, aluminium salt and manganese salt sum is the solution of 0.5～2mol/L; Described nickel salt is nickelous sulfate or nickel nitrate, and described cobalt salt is cobaltous sulfate or cobalt nitrate, and described aluminium salt is aluminum sulfate or aluminum nitrate, and described manganese salt is manganese sulfate or manganese nitrate;
(3) by weight be 1:(10～20) ratio, the liquid that step (1) is obtained joins in the solution of step (2) acquisition, stirs 1～3 hour;
(4) under agitation, with 15～30 hours, adding concentration in the liquid that step (3) obtains was lithium hydroxide aqueous solution or the sodium hydrate aqueous solution of 1～8mol/L, and making the pH value is 10～13, makes (the Ni of generation
0.8Co
0.15Al
0.03Mn
0.02) (OH)
2Even laminating is deposited to spherical reticle surface, leaves standstill to wear out in 24～48 hours, forms spherical presoma;
(5) be that 9～11 ammoniacal liquor fully washs with presoma pH, remove lithium ion or sodium ion, and sulfate ion or nitrate ion, in the 1mol presoma: the ratio of 100～1000 ml distilled waters, being scattered in the distilled water, is the ratio of 100:80 in the mol ratio with nickel salt, adds lithium hydroxide, dissolving is even, and spray drying is made the presoma that lithium hydroxide evenly coats;
(6) presoma that evenly coats of the lithium hydroxide that step (5) is obtained, 700～900 ℃ of calcining at constant temperature 12～48 hours, the content of constant temperature stage oxygen was 40%-65%; With cooling rate is that 3～10 ℃/minute speed is cooled to room temperature, pulverizes through airslide disintegrating mill, through grader classification, the quaternary anode material for lithium-ion batteries LiNi that obtains having spherical morphology
0.8Co
0.15Al
0.03Mn
0.02O
2
3. the preparation method of a kind of quaternary anode material for lithium-ion batteries according to claim 2 is characterized in that described mineral oil is No. 10 machine oil or No. 20 machine oil.
4. the preparation method of a kind of quaternary anode material for lithium-ion batteries according to claim 2 is characterized in that described non-ionic surface active agent is: APES, AEO or polyoxyethylene carboxylate.
5. the preparation method of a kind of quaternary anode material for lithium-ion batteries according to claim 2 is characterized in that described defoamer is a dimethicone.
6. the preparation method of a kind of quaternary anode material for lithium-ion batteries according to claim 2 is characterized in that described anticorrisive agent is sorbierite or benzoic acid.
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