CN103490051B - One is applicable to high-tension multielement cathode lithium electric material and preparation method thereof - Google Patents

One is applicable to high-tension multielement cathode lithium electric material and preparation method thereof Download PDF

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CN103490051B
CN103490051B CN201310428398.4A CN201310428398A CN103490051B CN 103490051 B CN103490051 B CN 103490051B CN 201310428398 A CN201310428398 A CN 201310428398A CN 103490051 B CN103490051 B CN 103490051B
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lithium
doped
multielement
solution
cobalt
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CN201310428398.4A
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CN103490051A (en
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高玉煙
徐频
石谦
陈东州
林宁
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成都晶元新材料技术有限公司
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection 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
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505Selection 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
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The present invention is that one is applicable to high-tension multielement cathode lithium electric material and preparation method thereof.This multielement cathode lithium electric material is individual particle pattern, and domain size distribution is 0.5-15 μm, adopts the nickel-cobalt-manganmultielement multielement lithium ion battery positive electrode material of composite mixed element, and chemical formula is LiNi xco ymn zm an bo 2in formula, the span of x, y, z is: 0.2≤x≤0.9,0≤y≤0.4,0.1≤z≤0.5,0 < a+b=1-x-y-z≤0.05, in formula, M is any one in titanium, aluminium, iron, vanadium, silicon, fluorine, group of the lanthanides, actinides, and N is any one in calcium, magnesium, aluminium, zirconium, iron, titanium.The present invention is on the basis of preparing the polynary lithium ion anode material of individual particle, adopt the method for composite mixed element-specific, under the prerequisite not changing chemical property own, promote the structural stability under high voltage discharge and recharge, effectively promote the cycle performance of material.

Description

One is applicable to high-tension multielement cathode lithium electric material and preparation method thereof

Technical field

The present invention relates to anode material for lithium-ion batteries preparation field, be specially one and be applicable to high-tension multielement cathode lithium electric material and preparation method thereof.

Background technology

At present, lithium ion battery, owing to having the features such as voltage is high, energy density is high, have extended cycle life, is widely used in the portable electric appts such as mobile phone, notebook computer, digital camera.In recent years, various electronic product is gradually to miniaturized, intelligent and functional diversities development, and this has higher requirement to the energy density of lithium ion battery.

Improving the charging voltage of battery, can significantly improve the capacity of battery under the condition not increasing active material in battery, is one of most effective way improving battery energy density.But, in high voltage cyclic process, because the lithium ion deviate from is too much, layer structure as the cobalt acid lithium of main flow positive active material is very unstable, especially, in charging process, there is lithium concentration gradient in cobalt acid lithium particle, grain surface layer lithium concentration is very low, very easy recurring structure subsides, and causes the cycle performance severe exacerbation of battery.Now safer, more cheap LiNi 0.5co 0.2mn 0.3o 2become the focus of positive electrode development gradually.

But nickle cobalt lithium manganate polynary positive pole material still has self-defect, particularly under high voltages, interface is because there is the existence of free lithium, with the poor compatibility of electrolyte, cause cycle performance not good, and existing lithium ion polynary positive pole material mostly is polycrystalline structure, structure is unstable under high voltages, more exacerbate the reaction with electrolyte, cycle performance is worsened.Therefore, the patent No. is that CN200810046300.8 discloses " a kind of nickel-cobalt-manganese multi-doped lithium ion battery cathode material and preparation method thereof ", prepare non-agglomerated individual particle material, improve the stability of particle discharge and recharge under high voltages, but still because the free lithium of layer structure and remained on surface, and cause the deterioration of circulation.Therefore need to carry out material modification to this polynary lithium ion anode material, comprise coating and doping.Comparatively speaking, doping means are more easily prepared and are not introduced complicated preparation section.Doped chemical can play the effect of bracing reinforcement to layer structure, and to a certain degree can the side reaction of lightening material and electrolyte.

Summary of the invention

The present invention just for above-mentioned Problems existing, provide a kind of meet make high-voltage lithium ion batteries requirement be applicable to high-tension multielement cathode lithium electric material and preparation method thereof.

The technical solution used in the present invention is such:

One is applicable to high-tension multielement cathode lithium electric material, and this multielement cathode lithium electric material is individual particle pattern, and domain size distribution is 0.5-15 μm, adopts the nickel-cobalt-manganmultielement multielement lithium ion battery positive electrode material of composite mixed element, and chemical formula is LiNi xco ymn zm an bo 2in formula, the span of x, y, z is: 0.2≤x≤0.9,0≤y≤0.4,0.1≤z≤0.5,0 < a+b=1-x-y-z≤0.05, in formula, M is any one in titanium, aluminium, iron, vanadium, silicon, fluorine, group of the lanthanides, actinides, and N is any one in calcium, magnesium, aluminium, zirconium, iron, titanium.

The preparation method of multielement cathode lithium electric material, comprises the following steps:

(1) NaOH and NH is joined in proportion by the mixing salt solution of nickel, cobalt, manganese and doped with the soluble salt solutions of M element 3mixed-alkali solution in, adjusted to ph is 7-10, forms suspension after stirring 1-5h at the temperature of 30-80 DEG C, then by the suspension filtered washing formed, dry and obtain doped with the intermediate Ni of the polynary positive pole material of M element xco ymn zm a(OH) 2;

(2) by the intermediate of the obtained polynary positive pole material doped with M element, be Li:(Ni+Co+Mn in molar ratio) ratio of=1-1.12:1 and lithium salts mixing, lithium salts is the one in lithium hydroxide, lithium carbonate or lithium nitrate, and add and mix doped with the oxide of N element or volatile salt, grinding 1-8h, low temperature presintering 1-5h at 350-550 DEG C; The PVAC polyvinylalcohol solution that concentration is 1-10% is added in the material after presintering, PVA solution consumption by percentage to the quality, account for the 10-20% of quality of material after presintering, in the roasting temperature 10-25h of 800-1000 DEG C after mixing, come out of the stove and be cooled to room temperature, namely obtain the individual particle structure nickel-cobalt-manganmultielement multielement lithium ion battery positive electrode material doped with M.

The mixed-alkali solution used in described step (1) is NaOH and NH 3mixed solution, the pH value > 8 of alkaline solution, wherein in mixed-alkali solution, the molar concentration of NaOH is 0.2-0.9mol/L, NH 3molar concentration be 0.1-0.9mol/L, the consumption of mixed-alkali solution is the intermediated chemistry formula Ni by the polynary positive pole material doped with M element xco ymn zm a(OH) 2the 1-1.07 of the molal quantity calculated doubly.

In described step (1) institute use that the soluble salt solutions of the mixing salt solution of nickel, cobalt, manganese and M element of adulterating is sulfate, one or more mixture in nitrate, chlorate, total metal molar concentration is 0.5-1.5mol/L, and in this metal salt solution, the mol ratio of nickel cobalt manganese and doping M element is by polynary anode material for lithium-ion batteries finished chemical formula configuration.

In described step (2) use the intermediate Ni of oxide doped with N element or volatile salt and the polynary positive pole material doped with M element xco ymn zm a(OH) 2mol ratio is by polynary anode material for lithium-ion batteries finished chemical formula configuration.

The invention has the beneficial effects as follows:

(1) on the basis of preparing the polynary lithium ion anode material of individual particle, the method for composite mixed element-specific is adopted.And be different from common doping way, the present invention's composite mixed point of two kinds of forms: a kind of by acid element doping at intracell, form distortional strain energy, make structure more stable; A kind of will be that the element doping of alkalescence is on crystal top layer, the nickel element of Substitute For Partial instability, the side reaction of suppression and electrolyte, under the prerequisite not changing chemical property own, promote the structural stability under high voltage discharge and recharge, effectively promote the cycle performance of material.

(2) this preparation method's doping is less, and does not substantially change original preparation technology, is easy to control, and production cost is low, easy to utilize.The product adopting the inventive method to prepare can be widely used in the new energy devices such as traditional lithium-ion battery, ultracapacitor, has a extensive future.

Accompanying drawing explanation

Fig. 1 is the SEM figure of the nickel-cobalt-manganmultielement multielement lithium ion battery positive electrode material containing doped chemical under this technique.

Fig. 2 is containing the nickel-cobalt-manganmultielement multielement lithium ion battery positive electrode material of doped chemical and the XRD comparison diagram of common individual particle multicomponent material under this technique.

Fig. 3 is nickel-cobalt-manganmultielement multielement lithium ion battery positive electrode material containing doped chemical and the charging and discharging curve of common individual particle multicomponent material under 3-4.35V charging/discharging voltage and 0.2C charging and discharging currents.

Fig. 4 is nickel-cobalt-manganmultielement multielement lithium ion battery positive electrode material containing doped chemical and the cyclic curve of common individual particle multicomponent material under 3-4.35V charging/discharging voltage and 1C charging and discharging currents.

Wherein a is common 523 type individual particle polynary positive pole materials, b is the individual particle polynary positive pole material of the common doped Ti element of 523 type, c is 523 type individual particle polynary positive pole materials of doped Ti, Al element, and d is the 523 type individual particle polynary positive pole materials of doped with Mg, Al.

Embodiment

In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.

Embodiment 1:

By the nickelous sulfate containing Ni element 19.57g, containing the cobaltous sulfate of Co element 19.64g, the manganese sulfate containing Mn element 18.18g, Titanium Nitrate containing the 0.53g of Ti element is dissolved in 1L pure water, stirring and dissolving, be configured to the multi-element metal salting liquid of total metal molar concentration 1.0mol/L, in this solution, the mol ratio of nickel cobalt manganese is Ni:Co:Mn=5:2:3.

Above-mentioned solution is heated to 70 DEG C, joins under agitation in 1.7L alkaline solution, react.This alkaline solution NH 3content is 0.6mol/L, NaOH content is 0.8mol/L.Adjusted to ph is 8.5, continues to stir 1h, filter, obtain solid content, with pure water material, be then placed in baking oven 110 DEG C of dry 5h after leaving standstill 2h after reinforced end, must doped with the intermediate of the polynary positive pole material of Ti.

By composite multi-component intermediate and 40.59gLiCO 3abundant mixing, in 550 DEG C of preliminary treatment 1h, again above-mentioned pretreated material is mixed with 9.85gPVA solution (accounting for 11% of pretreated material mass percentage), then baking furnace is placed in, roasting 10h at 1000 DEG C, come out of the stove, be cooled to normal temperature, cross 200 mesh sieve screenings after pulverizing, screenings is the micropore individual particle structure polynary positive pole material of doped Ti element.

The individual particle structure polynary positive pole material of doped Ti element prepared by the present embodiment, testing its particle size distribution by laser particle analyzer is 0.5-15 μm.After this material is made pole piece, tested by battery performance test instrument, under the discharge and recharge deboost of 3-4.35V, its chemical property 0.2C specific discharge capacity is 172.2mAh/g, 1C specific discharge capacity is 169.5mAh/g, and 30 weeks circulation specific discharge capacities are 160.0mAh/g.

Embodiment 2:

Nickel nitrate containing Ni element 29.35g, the cobalt nitrate containing Co element 11.74g, the manganese nitrate containing Mn element 16.48g and the Titanium Nitrate containing Ti element 0.57g are dissolved in 1.5L pure water, stirring and dissolving, be configured to the multi-element metal salting liquid of total metal molar concentration 1.5mol/L, in this solution, the mol ratio of nickel cobalt manganese is Ni:Co:Mn=5:2:3.

Above-mentioned solution is heated to 50 DEG C, joins under agitation in 1.5L alkaline solution and react, this alkaline solution NH 3content is 0.4mol/L, NaOH content is 0.9mol/L.Adjusted to ph is 8.0, continues to stir 4h, filter, obtain solid content, with pure water material, be then placed in baking oven 110 DEG C of dry 5h, obtain composite multi-component intermediate after leaving standstill 2h after reinforced end.

By composite multi-component intermediate and 43.08gLiOHH 2o and 0.18g nanometer Al 2o 3abundant mixing, in 350 DEG C of preliminary treatment 4h, again above-mentioned pretreated material is mixed with 12.86gPVA solution (accounting for 15% of pretreated material mass percentage), then baking furnace is placed in, roasting 18h at 900 DEG C, come out of the stove, be cooled to normal temperature, cross 200 mesh sieve screenings after pulverizing, screenings is the individual particle structure polynary positive pole material of doped Ti and Al element.

Individual particle structure polynary positive pole material prepared by the present embodiment, its particle size distribution is 0.7-20 μm, and chemical property 0.2C specific discharge capacity is 180.8mAh/g, 1C specific discharge capacity is 173.5mAh/g, and 30 weeks circulation specific discharge capacities are 162.2mAh/g.

Embodiment 3:

Nickel chloride containing Ni element 29.47g, the cobalt chloride containing Co element 11.72g, the manganese chloride containing Mn element 16.52g and the magnesium nitrate containing Mg element 0.12g are dissolved in 1.2L pure water, stirring and dissolving, be configured to the multi-element metal salting liquid of total metal molar concentration 1.2mol/L, in this solution, the mol ratio of nickel cobalt manganese is Ni:Co:Mn=5:2:3.

Above-mentioned solution is heated to 60 DEG C, joins under agitation in 2L alkaline solution, react, this alkaline solution NH 3content is 0.2mol/L, NaOH content is 0.5mol/L.Adjusted to ph is 9.0, continues to stir 3h, filter, obtain solid content, with pure water material, be then placed in baking oven 110 DEG C of dry 5h, obtain composite multi-component intermediate after leaving standstill 2h after reinforced end.

By composite multi-component intermediate and 41.94gLiOHH 2o and 0.21g nanometer Al 2o 3abundant mixing, in 400 DEG C of preliminary treatment 2h, again above-mentioned pretreated material is mixed with 16.68gPVA solution (accounting for 18% of the mass percentage of pretreated material), then baking furnace is placed in, roasting 20h at 880 DEG C, come out of the stove, be cooled to normal temperature, cross 200 mesh sieve screenings after pulverizing, screenings is the individual particle structure polynary positive pole material of doped with Mg and Al element.

This profile is the polynary positive pole material of individual particle structure, and its particle size distribution is 0.7-15 μm, and chemical property 0.2C specific discharge capacity is 179.0mAh/g, 1C specific discharge capacity is 170.6mAh/g, and 30 weeks circulation specific discharge capacities are 165.3mAh/g.

Comparative example 1:

In example 2, keep other parameter constants, changing sintering temperature in baking furnace is 720 DEG C.The powder body material finally obtained is through X-ray diffraction (XRD) and ESEM (SEM) test, and what draw is not the individual particle structure polynary positive pole material that degree of crystallinity is intact.And chemical property extreme difference, 0.2C specific discharge capacity is only 75.3mAh/g, and 1C specific discharge capacity is 42.6mAh/g, cannot carry out circulation discharge test because capacity is too low.

Comparative example 2:

In embodiment 3, keep other parameter constants, changing the quality adding magnesium nitrate is 2.31g.The individual particle structure polynary positive pole material being doped Ti and Al element finally obtained, but can be found out by XRD test, this material XRD collection of illustrative plates has the dephasign peak of obvious MgO.By electrochemical property test, to obtain 0.2C specific discharge capacity be 157.8mAh/g, 1C specific discharge capacity is 135.3mAh/g, and within 30 weeks, circulation specific discharge capacity is 95.7mAh/g, and charge-discharge performance is poor.

Claims (4)

1. be applicable to a preparation method for high-tension multielement cathode lithium electric material, it is characterized in that comprising the following steps:
(1) NaOH and NH is joined in proportion by the mixing salt solution of nickel, cobalt, manganese and doped with the soluble salt solutions of M element 3mixed-alkali solution in, adjusted to ph is 7-10, forms suspension after stirring 1-5h at the temperature of 30-80 DEG C, then by the suspension filtered washing formed, dry and obtain doped with the intermediate Ni of the polynary positive pole material of M element xco ymn zm a(OH) 2;
(2) by the intermediate of the obtained polynary positive pole material doped with M element, be Li in molar ratio:
(Ni+Co+Mn) ratio of=1-1.12:1 and lithium salts mixing, lithium salts is the one in lithium hydroxide, lithium carbonate or lithium nitrate, and add and mix doped with the oxide of N element or volatile salt, grinding 1-8h, low temperature presintering 1-5h at 350-550 DEG C; The PVAC polyvinylalcohol solution that concentration is 1-10% is added in the material after presintering, PVA solution consumption by percentage to the quality, account for the 10-20% of quality of material after presintering, in the roasting temperature 10-25h of 800-1000 DEG C after mixing, come out of the stove and be cooled to room temperature, namely the individual particle structure nickel-cobalt-manganmultielement multielement lithium ion battery positive electrode material doped with M element and N element is obtained
Wherein, described multielement cathode lithium electric material is individual particle pattern, and domain size distribution is 0.5-15 μm, adopts the nickel-cobalt-manganmultielement multielement lithium ion battery positive electrode material of composite mixed element, and chemical formula is LiNi xco ymn zm an bo 2in formula, the span of x, y, z is: 0.2≤x≤0.9,0≤y≤0.4,0.1≤z≤0.5,0 < a+b=1-x-y-z≤0.05, in formula, M is any one in titanium, aluminium, iron, vanadium, silicon, fluorine, group of the lanthanides, actinides, and N is any one in calcium, magnesium, aluminium, zirconium, iron, titanium.
2. the preparation method being applicable to high-tension multielement cathode lithium electric material according to claim 1, is characterized in that: the mixed-alkali solution used in described step (1) is NaOH and NH 3mixed solution, the pH value > 8 of alkaline solution, wherein in mixed-alkali solution, the molar concentration of NaOH is 0.2-0.9mol/L, NH 3molar concentration be 0.1-0.9mol/L, the consumption of mixed-alkali solution is the intermediated chemistry formula Ni by the polynary positive pole material doped with M element xco ymn zm a(OH) 2the 1-1.07 of the molal quantity calculated doubly.
3. the preparation method being applicable to high-tension multielement cathode lithium electric material according to claim 1, it is characterized in that: institute uses the mixing salt solution of nickel, cobalt, manganese and the soluble salt solutions of M element of adulterating is one or more mixture in its sulfate, nitrate, chlorate in described step (1), total metal molar concentration is 0.5-1.5mol/L, and in this metal salt solution, the mol ratio of nickel cobalt manganese and doping M element is by polynary anode material for lithium-ion batteries finished chemical formula configuration.
4. the preparation method being applicable to high-tension multielement cathode lithium electric material according to claim 1, is characterized in that: in described step (2) use the intermediate Ni of oxide doped with N element or volatile salt and the polynary positive pole material doped with M element xco ymn zm a(OH) 2mol ratio is by polynary anode material for lithium-ion batteries finished chemical formula configuration.
CN201310428398.4A 2013-09-18 2013-09-18 One is applicable to high-tension multielement cathode lithium electric material and preparation method thereof CN103490051B (en)

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