CN105826531A - Preparation method for in-situ carbon-coated lithium nickel manganese oxide anode material and product thereof - Google Patents
Preparation method for in-situ carbon-coated lithium nickel manganese oxide anode material and product thereof Download PDFInfo
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- CN105826531A CN105826531A CN201610175985.0A CN201610175985A CN105826531A CN 105826531 A CN105826531 A CN 105826531A CN 201610175985 A CN201610175985 A CN 201610175985A CN 105826531 A CN105826531 A CN 105826531A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method for an in-situ carbon-coated lithium nickel manganese oxide anode material and a product thereof. The preparation method comprises the following steps that S1, lithium (Li) salt, nickel (Ni) salt and manganese (Mn) salt are dissolved in deionized water to form a solution A, and the total concentration of metal ions in the solution A ranges from 0.1 mol/L to 1 mol/L; S2, resorcinol and a formaldehyde solution are mixed to be uniform to form a solution B; S3, the solution A and the solution B are mixed to be uniform, injected in a reactor, heated to 70-90 DEG C after sealing, and aged to form solid sol; S4, the solid sol is dried and then roasted at high temperature under the protection of inert gas. According to the preparation method, by optimally selecting precursors (resorcinol and formaldehyde) of the carbon-coated material and strictly controlling the dosage relation between all components, eventually the surface of lithium nickel manganese oxide is coated with carbon uniformly. By the adoption of the method, the tolerance of the lithium nickel manganese oxide anode material to an electrolyte is improved, and meanwhile the cyclic stability of the material can be improved.
Description
Technical field
The present invention relates to technical field of lithium ion, be coated with preparation method of nickel lithium manganate cathode material and products thereof more particularly, to a kind of in-situ carbon.
Background technology
Lithium ion battery developing direction is high-energy-density, high power and long-life at present.Positive electrode, as the core component of lithium ion battery, is the research and development keys with lithium ion battery with high energy density of new generation.Compared with the positive electrode of other business application, nickel ion doped (LiNi0.5Mn1.5O4) because the theoretical discharge capacity of the removal lithium embedded plateau potential and 146.7mAh/g with about 4.7V is it is considered to be have most the high-voltage anode material of application prospect.
Positive electrode surface directly contacts with electrolyte, the Mn in nickel ion doped material in charge and discharge process3+It is easily soluble in electrolyte molten, and the electric conductivity of nickel ion doped is poor, stock utilization is low, Li+Diffusion impedance is big, and the reversibility thus causing battery is poor, the capacity attenuation problem such as seriously in cyclic process.For solving this difficult problem, there is research worker at LiNi0.5Mn1.5O4Adulterate in material the metallic elements such as Cr, Mg, Ni, Ti, is combined with O and forms the chemical bond more more stable than Mn-O bond energy to stablize LiNi0.5Mn1.5O4Lattice structure, with suppression because of Mn3+Dissolve the nickel ion doped lattice caused to subside.
It addition, research worker is attempted at LiNi0.5Mn1.5O4The protection material that the Surface coating of material is inert to electrolyte, to reduce the metal ion Oxidation to electrolyte of high-valence state so that electrolyte is more stable, can stop Mn simultaneously3+Dissolution.
But current technology still cannot effective particle surface protective mulch equably to nickel ion doped material, to reach above-mentioned purpose, thus effectively extend the material even service life of battery.
Summary of the invention
The present invention is to overcome the defect described in above-mentioned prior art, it is provided that the preparation method of a kind of in-situ carbon cladding nickel lithium manganate cathode material.
For solving above-mentioned technical problem, the technical solution used in the present invention is:
The preparation method of a kind of in-situ carbon cladding nickel lithium manganate cathode material, comprises the following steps:
S1. lithium (Li) salt, nickel (Ni) salt, manganese (Mn) salt being dissolved in deionized water, form solution A, in solution A, the total concentration of metal ion is 0.1 ~ 1mol/L；
S2. by resorcinol and formalin mix homogeneously, solution B is formed；The weight sum of described resorcinol and formaldehyde accounts for the 25 ~ 60% of the weight of described solution B；
S3., by solution A and solution B mix homogeneously, in injecting reactor, sealing post-heating is to 70 ~ 90 DEG C, aging, forms solid sols；
S4. solid sols is dried, then under the protection of noble gas, high-temperature roasting, i.e. obtain the nickel lithium manganate cathode material of in-situ carbon cladding.
Described solution A is the precursor solution of nickel ion doped, and by adding the precursor of carbon encapsulated material in the precursor solution of described nickel ion doped, two kinds of solution are effectively mixed, and by the precursor (resorcinol and formaldehyde) of preferred carbon encapsulated material, strictly control each component uses magnitude relation, finally make carbon be evenly coated on the surface of nickel ion doped, thus effectively extend the material even service life of battery.
Preferably, described solution A is 1.5 ~ 2.5:1, preferably 2:1 with the volume ratio of solution B.
Described lithium salts, nickel salt, manganese salt can be used the existing middle respective metal salt preparing nickel ion doped, it is preferred to use Quilonorm (SKB), nickel acetate, manganese acetate.
Preferably, in described solution A, the total concentration of metal ion is 0.4 ~ 0.8mol/L, more preferably 0.6mol/L.
Preferably, in described solution A, the mol ratio of Li, Ni, Mn is 2:1:3.
Preferably, in described solution B, the weight sum of described resorcinol and formaldehyde accounts for the 45 ~ 60% of the weight of described solution B.
Preferably, in described solution B, resorcinol is 1:1.5 ~ 2.5, more preferably 1:2 with the mol ratio of formaldehyde.
Preferably, in step S3, the described aging time is 3 ~ 10 days, more preferably 6 ~ 8 days.
Preferably, in step S4, described be dried into vacuum drying, be dried temperature be 70 ~ 130 DEG C.
In step S4, the condition of described high-temperature roasting is roasting 10 ~ 15 hours at 450 ~ 900 DEG C, preferably roasting 10 ~ 15 hours at 800 ~ 900 DEG C, more preferably 850 ~ 880 DEG C.
It is a further object of the invention to provide a kind of by above-mentioned preparation method preparation-obtained in-situ carbon cladding nickel lithium manganate cathode material.
Additionally also providing for a kind of lithium ion battery, it includes positive pole, and described positive pole uses above-mentioned in-situ carbon cladding nickel lithium manganate cathode material to be prepared from.
Compared with prior art, the invention has the beneficial effects as follows:
The method that the present invention uses in-situ carbon to be coated with carries out carbon cladding to nickel ion doped, and by the precursor (resorcinol and formaldehyde) of preferred carbon encapsulated material, strictly control each component uses magnitude relation, finally make carbon be evenly coated on the surface of nickel ion doped.After using the method, the toleration of electrolyte is improved by nickel lithium manganate cathode material, can also improve the stable circulation performance of material simultaneously.
Accompanying drawing explanation
Fig. 1 is the charging and discharging curve figure of embodiment 1 and the preparation-obtained battery of comparative example.
Fig. 2 is the cycle performance curve chart of embodiment 1 and the preparation-obtained battery of comparative example.
Fig. 3 embodiment 1 and the X-ray diffractogram of the preparation-obtained material of comparative example.
Detailed description of the invention
Further describe the present invention by specific examples below, it will be appreciated that specific embodiment described herein is only used for explaining the present invention, is not intended to limit the present invention, various change can be carried out in the range of right of the present invention limits.
Embodiment 1
The preparation of in-situ carbon cladding nickel lithium manganate cathode material
S1. being that 2:1:3 weighs Quilonorm (SKB), nickel acetate, manganese acetate according to the mol ratio of Li, Ni, Mn, and be dissolved in deionized water, forming solution A, in solution A, the total concentration of metal ion is 0.6mol/L.
S2. by resorcinol and formalin mix homogeneously, formation solution B, the weight sum that mol ratio is 1:2, resorcinol and formaldehyde of resorcinol and formaldehyde accounts for the 55% of the weight of solution B；
S3. it is 2:1 mix homogeneously by volume by solution A and solution B, injects in autoclave, seal post-heating to 85 DEG C, aging 7 days, form tan solid sols.
S4. being taken out from autoclave by solid sols, at 90 DEG C, vacuum (-0.08MPa) is dried 24 hours, then under the protection of noble gas, at N2Protect lower 800 DEG C of high-temperature roastings 12 hours, obtain the nickel lithium manganate cathode material of in-situ carbon cladding, grind standby.
The preparation of test battery
By appropriate Kynoar (PVDF) in N-Methyl pyrrolidone (NMP) stirring and dissolving, sonic oscillation 10min, add preparation-obtained nickel lithium manganate cathode material and acetylene black, nickel ion doped: acetylene black: PVDF=80:10:10(mass ratio), stir 3 hours, obtain modest viscosity, finely dispersed slurry, be coated on aluminium foil, obtain pole piece.
Then pole piece is dried 2 hours in 90 DEG C of air dry ovens, is then transferred to vacuum (-0.08MPa) in 110 DEG C of vacuum drying ovens and is dried 12 hours.In the pole piece roll squeezer that will be dried after roll-in, it is cut into the little pole piece of a diameter of 10mm, is placed again into little pole piece in 120 DEG C of vacuum drying ovens being dried and weighs for 3 hours, then be transferred in the glove box of full high-purity argon gas standby.With lithium sheet as negative pole in glove box, being assembled into the 2032 button-shaped half-cells of type, electrolyte is 1MLiPF6/EC+DMC (1:1, mass ratio).
The assembling sequence of button cell assembling is: negative cover-spring leaf-stainless steel substrates-cathode of lithium-electrolyte-barrier film-electrolyte-positive plate (collector is just to positive cover)-positive cover, all parts is neatly folded, will test after battery pressurization with sealing machine.
Charge-discharge performance is tested
Above-mentioned battery is carried out charge-discharge test under conditions of 0.5C multiplying power, discharge and recharge interval are 3.5 ~ 5.0V, Fig. 1 is the charging and discharging curve figure of its second circle, as seen from Figure 2, after carbon surface cladding, battery is improved at the specific discharge capacity of 4.7V charge and discharge platform, and the second circle specific discharge capacity is brought up to 134mAh/g by 124mAh/g time uncoated.
Cycle performance is tested
Above-mentioned battery is circulated performance test under 0.5C multiplying power, as shown in Figure 2.
This enforcement preparation-obtained in-situ carbon cladding nickel ion doped material then shows extraordinary cyclical stability, and after 100 times circulate, charging and discharging capacity is only reduced to 130mAh/g from 135mAh/g, and capability retention reaches 96.3%.
Comparative example
Weigh Quilonorm (SKB), nickel acetate, manganese acetate according to the usage ratio of embodiment 1, and prepare according to conventional nickel ion doped preparation method, at 800 DEG C, calcine 12h, obtain LiNi0.5Mn1.5O4。
Preparing of test battery is same as in Example 1.
Above-mentioned battery carries out under 0.5C multiplying power charge-discharge performance test and cycle performance test, and method of testing is same as in Example 1, and result is as shown in Figure 2.
After 100 times circulate, the charging and discharging capacity of the preparation-obtained battery of comparative example is reduced to 88mAh/g from 124mAh/g, and capability retention reaches 70.4%.
Embodiment 2 ~ 8
The preparation process of embodiment 2 ~ 8 is same as in Example 1 with preparing of test battery, is with the difference of embodiment 1, metal ion total concentration, resorcinol and the mol ratio of formaldehyde and resorcinol and the percentage composition of formaldehyde, as shown in table 1.
Table 1
Above-described embodiment and comparative example are circulated performance test, and the method for test is same as in Example 1, and its result is as shown in table 2.
Table 2
X-ray diffraction detects
Material preparation-obtained to embodiment 1 and comparative example carries out X-ray diffraction detection, and its result is as shown in Figure 3.
As seen from Figure 3, the crystalline structure of nickel ion doped material is not had much affect by carbon cladding, and in-situ carbon cladding nickel ion doped still has the spinel structure that space group is Fd3m, and the nickel ion doped material after being coated with has more preferable degree of crystallinity.
Obviously, the above embodiment of the present invention is only for clearly demonstrating example of the present invention, and is not the restriction to embodiments of the present invention.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also cannot all of embodiment be given exhaustive.All any amendment, equivalent and improvement etc. made within the spirit and principles in the present invention, within should be included in the protection domain of the claims in the present invention.
Claims (9)
1. the preparation method of an in-situ carbon cladding nickel lithium manganate cathode material, it is characterised in that comprise the following steps:
S1. lithium (Li) salt, nickel (Ni) salt, manganese (Mn) salt being dissolved in deionized water, form solution A, in solution A, the total concentration of metal ion is 0.1 ~ 1mol/L；
S2. by resorcinol and formalin mix homogeneously, solution B is formed；The weight sum of described resorcinol and formaldehyde accounts for the 25 ~ 60% of the weight of described solution B；
S3., by solution A and solution B mix homogeneously, in injecting reactor, sealing post-heating is to 70 ~ 90 DEG C, aging, forms solid sols；
S4. solid sols is dried, then under the protection of noble gas, high-temperature roasting, i.e. obtain the nickel lithium manganate cathode material of in-situ carbon cladding.
Preparation method the most according to claim 1, it is characterised in that in described solution A, the total concentration of metal ion is 0.4 ~ 0.8mol/L.
Preparation method the most according to claim 1, it is characterised in that in described solution A, the mol ratio of Li, Ni, Mn is 2:1:3.
Preparation method the most according to claim 1, it is characterised in that in described solution B, the weight sum of described resorcinol and formaldehyde accounts for the 45 ~ 60% of the weight of described solution B.
Preparation method the most according to claim 1, it is characterised in that in described solution B, resorcinol and formaldehyde mole ratio be 1:1.5 ~ 2.5.
Preparation method the most according to claim 1, it is characterised in that in step S4, described be dried into vacuum drying, be dried temperature be 70 ~ 130 DEG C.
Preparation method the most according to claim 1, it is characterised in that in step S4, the condition of described high-temperature roasting is roasting 10 ~ 15 hours at 450 ~ 900 DEG C.
8. an in-situ carbon cladding nickel lithium manganate cathode material, it is characterised in that use the preparation method described in any one of claim 1 ~ 7 to prepare.
9. a lithium ion battery, it is characterised in that include positive pole, described positive pole uses the in-situ carbon cladding nickel lithium manganate cathode material described in claim 8 to be prepared from.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107017391A (en) * | 2017-04-18 | 2017-08-04 | 深圳市集创云天新材料有限公司 | Core shell structure anode composite material and preparation method thereof, lithium ion battery |
| CN108899506A (en) * | 2018-07-03 | 2018-11-27 | 广州大学 | A kind of porous nano carbon coating manganate cathode material for lithium and preparation method thereof |
| CN112186158A (en) * | 2020-09-28 | 2021-01-05 | 蜂巢能源科技有限公司 | Positive electrode composite material and preparation method and application thereof |
| CN113666432A (en) * | 2021-07-30 | 2021-11-19 | 蜂巢能源科技有限公司 | Carbon-coated nickel-manganese binary cobalt-free positive electrode material, preparation method thereof and lithium ion battery |
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| CN104319370A (en) * | 2014-09-28 | 2015-01-28 | 洛阳理工学院 | Preparation method of LiNixCoyMnzO2 serving as ternary positive electrode material of lithium ion battery |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107017391A (en) * | 2017-04-18 | 2017-08-04 | 深圳市集创云天新材料有限公司 | Core shell structure anode composite material and preparation method thereof, lithium ion battery |
| CN108899506A (en) * | 2018-07-03 | 2018-11-27 | 广州大学 | A kind of porous nano carbon coating manganate cathode material for lithium and preparation method thereof |
| CN112186158A (en) * | 2020-09-28 | 2021-01-05 | 蜂巢能源科技有限公司 | Positive electrode composite material and preparation method and application thereof |
| CN113666432A (en) * | 2021-07-30 | 2021-11-19 | 蜂巢能源科技有限公司 | Carbon-coated nickel-manganese binary cobalt-free positive electrode material, preparation method thereof and lithium ion battery |
| CN113666432B (en) * | 2021-07-30 | 2022-12-09 | 蜂巢能源科技有限公司 | Carbon-coated nickel-manganese binary cobalt-free positive electrode material, preparation method thereof and lithium ion battery |
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