CN106299255A - A kind of preparation method of big particle diameter spinel nickel LiMn2O4 - Google Patents

A kind of preparation method of big particle diameter spinel nickel LiMn2O4 Download PDF

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CN106299255A
CN106299255A CN201610728117.0A CN201610728117A CN106299255A CN 106299255 A CN106299255 A CN 106299255A CN 201610728117 A CN201610728117 A CN 201610728117A CN 106299255 A CN106299255 A CN 106299255A
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ion doped
nickel ion
particle diameter
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CN106299255B (en
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樊少娟
杨立铭
汪涛
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Hefei Gotion High Tech Power Energy Co Ltd
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Hefei Guoxuan High Tech Power Energy Co Ltd
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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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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

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Abstract

A kind of preparation method of big particle diameter spinel-type nickel ion doped, high speed ball milling after the compound of Li, Ni and doped chemical M is mixed with certain chemical ratios, it is thus achieved that the homogeneous mixture A of Li, Ni, M；Lithium salts, nickel salt, manganese salt being dissolved in alcohol solvent according to the chemical ratios of 1:0.5:1.5, ammonia is adjusted to colloidal sol shape, obtains nickel ion doped sol B；The homogeneous mixture A of Li, Ni, M, nickel ion doped sol B and Mn oxide C mix and blend are mixed, is dried to obtain mixture D；Mixture D high temperature sintering is obtained nickel ion doped material.Nickel lithium manganate cathode material crystal grain prepared by the present invention is complete, and specific surface area is little, and bulk density is high, and high-low temperature cycle lifetime is excellent.

Description

A kind of preparation method of big particle diameter spinel nickel LiMn2O4
Technical field
The invention belongs to field of material technology, relate to the preparation method of a kind of anode material for lithium-ion batteries, particularly relate to A kind of preparation method of anode material for lithium-ion batteries big particle diameter spinel-type nickel ion doped.
Background technology
Along with worldwide energy scarcity and environmental requirement, electric automobile has become the developing direction of automobile industry. Electrokinetic cell, as the important component part of electric automobile, directly affects electric automobile performance.Power lithium-ion battery has work Make that voltage height, memory-less effect, self-discharge rate be little, energy density big become with cycle life notable the most a little, extensive application Prospect.And in terms of the security performance of power lithium-ion battery, positive electrode is the pass of limiting lithium ion electrokinetic cell development One of key factor.Seek high-energy-density, high safe and environment-friendly and low-cost electrode material is the emphasis side in current industry To.
The positive electrode commonly used at present is cobalt acid lithium, LiMn2O4, nickle cobalt lithium manganate, LiFePO4 and high electricity respectively Pressure nickel ion doped etc..Owing to cobalt is expensive, and cobalt acid lithium, nickle cobalt lithium manganate are bigger for the potential safety hazard of electrokinetic cell.Manganese Acid lithium, nickel ion doped and LiFePO4 are the positive electrodes that lithium-ion-power cell is ideal.Although lithium manganate material becomes This is the lowest, and security performance is good, but specific capacity is the most on the low side, due to Mn dissolving, Jahn-Teller distortion effect and lattice not Stable, cause cycle life especially high temperature cyclic performance undesirable.Research shows that doping can be effectively improved its high temperature circulation Can, the LiNi of especially Ni doping0.5Mn1.5O4So that the price of manganese is higher than 3.5, it is possible to effectively suppression Mn dissolves, Jahn- Teller distortion effect and the unstability of lattice, and discharge voltage plateau is up to 4.7V, becomes a preferable power Cell positive material.
Additionally, in order to improve cycle performance further, research shows to obtain the big grain of low specific surface area by controlling pattern Footpath nickel ion doped material, it is possible to significantly improve the high temperature cyclic performance of nickel ion doped.The nickel ion doped material of big particle diameter has low Specific surface area, decrease the contact area of material and electrolyte, can reduce the dissolving of manganese in electrolyte, improve product in electrolysis In stability, be effectively improved the cycle performance of battery.
Summary of the invention
It is an object of the present invention to provide the preparation method of a kind of big particle diameter spinel-type nickel ion doped, nickel manganese prepared by the present invention Acid lithium anode material crystal grain is complete, and specific surface area is little, and bulk density is high, and high-low temperature cycle lifetime is excellent.
Technical scheme is as follows:
The preparation method of a kind of big particle diameter spinel-type nickel ion doped, it is characterised in that comprise the steps:
(1) high speed ball milling after the compound of Li, Ni and doped chemical M being mixed with certain chemical ratios, it is thus achieved that Li, Ni, M's Homogeneous mixture A；
(2) lithium salts, nickel salt, manganese salt being dissolved in alcohol solvent according to the chemical ratios of 1:0.5:1.5, ammonia is adjusted to colloidal sol shape, Obtain nickel ion doped sol B；
(3) the homogeneous mixture A of Li, Ni, M, nickel ion doped sol B and Mn oxide C mix and blend are mixed, be dried to obtain mixed Compound D；
(4) mixture D high temperature sintering is obtained nickel ion doped material.
Preferably, in described step (1), the compound of Li, Ni, M is oxide, carbonate, nitrate, acetic acid The mixture of one or more in salt, oxalates or hydroxide.
Preferably, in described step (1), doped chemical M is nickel position or Mn-site doping, and be Al, Co, Cr, Zn, Y, One or both elements in Fe, Ag, Ca, V, Cu, Zr, Ti, Sn, Mo, La, Ce, Pr, Nd.
Preferably, in described step (1), the particle size range of homogeneous mixture A is 100nm～5 μm.
Preferably, in described step (2), lithium salts, nickel salt, manganese salt be nitrate, acetate, oxalates, carbonate or The mixture of one or more in hydroxide.
Preferably, in described step (3), the ratio adding nickel ion doped sol B is 1%～20%.
Preferably, in described step (3), Mn oxide C is particle diameter manganese dioxide in 5～15 μ m or four oxygen Change three manganese.
Preferably, in described step (3), the mixture of homogeneous mixture A, nickel ion doped sol B and Mn oxide C It is dried and is 70～100 DEG C and is dynamically dried.
Preferably, ratio a of described doped chemical M is in the range of 0 ＜ a≤0.5m, and wherein, m is institute's substitute element position Ratio.
Beneficial effects of the present invention is as follows:
The present invention by the compound micronization processes to Li, Ni and doped chemical M, and with micron order Mn oxide and nickel mangaic acid High-temperature calcination again after lithium colloidal sol combination drying, can control its average particle size particle size in 5～15 μm, and crystal grain is complete, high/low temperature Cycle life is excellent.Big particle diameter spinel-type nickel ion doped has low specific surface area, decreases contacting of material and electrolyte Area, can reduce the dissolving of manganese in electrolyte, improves product stability in electrolysis, is effectively improved the cycle performance of battery. The biggest particle diameter spinel-type nickel ion doped bulk density is high, it is provided that have the lithium battery of high-energy-density.
Accompanying drawing explanation
Fig. 1 is the SEM figure of big particle diameter spinel-type nickel ion doped prepared by the present invention；
Fig. 2 is the big particle diameter spinel-type nickel ion doped prepared of the present invention charging and discharging curve at 0.2C；
Fig. 3 is 1C cycle performance curve under big particle diameter spinel-type nickel ion doped room temperature prepared by the present invention.
Fig. 4 is 1C cycle performance curve at big particle diameter spinel-type nickel ion doped 55 DEG C prepared by the present invention.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in further detail, it is clear that described embodiment is only It is only a part of embodiment to the present invention, is not whole embodiments.Based on the embodiment in the present invention, this area general Other all embodiments that logical technical staff is obtained under not making creative work premise, broadly fall into the protection of the present invention Scope.
Embodiment 1:
A kind of big particle diameter spinel-type nickel ion doped LiNi0.45Mn1.45Fe0.1O4Synthesis, prepare in accordance with the following steps:
(this chemical ratios is known ratio, at this slightly to weigh the lithium carbonate of certain chemical ratios, nickel protoxide and Ferrox. Go), employing ethanol is grinding aid, and zirconium oxide is ball-milling medium, and ratio of grinding media to material is 5:1, and solid content is 60%, utilizes nanometer mill at a high speed Ball milling, obtains the homogeneous mixture that granularity D50 is about 500nm.Have another name called by the metering score of 1:0.5:1.5 and take lithium nitrate, nitre Acid nickel, manganese acetate are dissolved in alcohol solvent, then make it to colloidal sol shape with ammonia regulation PH, obtain nickel ion doped colloidal sol.By 5% Nickel ion doped colloidal sol, D50 be that the mangano-manganic oxide of 7 μm joins in aforesaid homogeneous mixture, open nanometer and grind and open Circulating pump, stirring at low speed 1h, 80 DEG C are dynamically dried.By first for the mixture after dry combustion method high-temperature calcination 12h at a temperature of 950 DEG C, then Anneal at a temperature of 700 DEG C 18h, i.e. obtains required big particle diameter spinel-type nickel ion doped LiNi0.45Mn1.45Fe0.1O4。
Fig. 1 is the SEM figure of big particle diameter spinel-type nickel ion doped, it can be seen that the nickel ion doped material particle size of preparation is at 5 μ About m, octahedra crystal grain is complete.The material of gained is used for electric performance test, and Fig. 2 is the charging and discharging curve of 0.2C, and capacity is 134mAh/g.Fig. 3 is 1C cyclic curve at 25 DEG C, it can be seen that 500 weeks capability retentions are more than 95%.Fig. 4 is 1C cyclic curve at 55 DEG C, as can be seen from the figure 200 weeks capability retentions are more than 90%.
Embodiment 2:
A kind of big particle diameter spinel-type nickel ion doped LiNi0.5Mn1.4Cr0.1O4Synthesis, prepare in accordance with the following steps:
(this chemical ratios is known ratio, at this slightly to weigh the lithium carbonate of certain chemical ratios, nickel protoxide and chromium oxide Go), employing ethanol is grinding aid, and zirconium oxide is ball-milling medium, and ratio of grinding media to material is 9:1, and solid content is 50%, utilizes nanometer mill at a high speed Stirring, obtains the homogeneous mixture that granularity D50 is about 200nm.Have another name called by the metering score of 1:0.5:1.5 and take lithium nitrate, second Acid nickel, manganese nitrate are dissolved in alcohol solvent, then make it to colloidal sol shape with ammonia regulation PH, obtain nickel ion doped colloidal sol.By 10% Nickel ion doped colloidal sol, D50 be that the mangano-manganic oxide of 10 μm joins in aforesaid homogeneous mixture, open nanometer and grind and open Circulating pump, stirring at low speed 1h, 80 DEG C are dynamically dried.By first for the mixture after dry combustion method high-temperature calcination 12h at a temperature of 850 DEG C, then Anneal at a temperature of 700 DEG C 10h, i.e. obtains required big particle diameter spinel-type nickel ion doped LiNi0.5Mn1.4Cr0.1O4.By institute The material obtained is for electric performance test, and 0.2C specific discharge capacity is 133mAh/g, and room temperature 1C 300 weeks capability retentions of circulation are More than 98%, high temperature 1C 200 weeks capability retentions of circulation are more than 92.
Embodiment 3:
A kind of big particle diameter spinel-type nickel ion doped LiNi0.45Mn1.5Ti0.05O4Synthesis, prepare in accordance with the following steps:
(this chemical ratios is known ratio, at this slightly to weigh the lithium carbonate of certain chemical ratios, nickel protoxide and titanium dioxide Go), employing ethanol is grinding aid, and zirconium oxide is ball-milling medium, and ratio of grinding media to material is 7:1, and solid content is 60%, utilizes nanometer mill at a high speed Stirring, obtaining granularity D50 is the homogeneous mixture about 1 μm.Have another name called by the metering score of 1:0.5:1.5 and take Lithium hydrate, nitre Acid nickel, manganese nitrate are dissolved in alcohol solvent, then make it to colloidal sol shape with ammonia regulation PH, obtain nickel ion doped colloidal sol.By 15% Nickel ion doped colloidal sol, D50 be that the manganese dioxide of 8 μm joins in aforesaid homogeneous mixture, open nanometer and grind and open and follow Ring pump, stirring at low speed 1h, 70 DEG C are dynamically dried.By first for the mixture after dry combustion method high-temperature calcination 12h at a temperature of 1000 DEG C, then Anneal at a temperature of 750 DEG C 18h, i.e. obtains required big particle diameter spinel-type nickel ion doped LiNi0.45Mn1.5Ti0.05O4.By institute The material obtained is for electric performance test, and 0.2C specific discharge capacity is 130mAh/g, and room temperature 1C 300 weeks capability retentions of circulation are More than 96%, high temperature 1C 200 weeks capability retentions of circulation are more than 90%.
Embodiment 4:
A kind of big particle diameter spinel-type nickel ion doped LiNi0.45Mn1.45Ti0.05Al0.05O4Synthesis, prepare in accordance with the following steps:
(this chemical ratios is known to weigh the lithium carbonate of certain chemical ratios, nickel protoxide, titanium dioxide and aluminium sesquioxide Ratio, omits at this), employing ethanol is grinding aid, and zirconium oxide is ball-milling medium, and ratio of grinding media to material is 3:1, and solid content is 55%, utilizes Nanometer mill high-speed stirred, obtains the homogeneous mixture that granularity D50 is about 800nm.Have another name called by the metering score of 1:0.5:1.5 and take Lithium hydrate, nickel nitrate, manganese nitrate are dissolved in alcohol solvent, then make it to colloidal sol shape with ammonia regulation PH, obtain nickel mangaic acid Lithium colloidal sol.Nickel ion doped colloidal sol by 20%, D50 are that the manganese dioxide of 5 μm joins in aforesaid homogeneous mixture, open and receive Rice mill ON cycle pump, stirring at low speed 1h, 80 DEG C are dynamically dried.By first for the mixture after dry combustion method high temperature at a temperature of 900 DEG C Calcining 12h, then the 12h that anneals at a temperature of 750 DEG C, i.e. obtain required big particle diameter spinel-type nickel ion doped LiNi0.45Mn1.45Ti0.05Al0.05O4.The material of gained is used for electric performance test, and 0.2C specific discharge capacity is 129mAh/g, often Temperature 1C 300 weeks capability retentions of circulation are more than 97%, and high temperature 1C 200 weeks capability retentions of circulation are more than 93%.
Embodiment 5:
A kind of big particle diameter spinel-type nickel ion doped LiNi0.45Mn1.45Cu0.1O4Synthesis, prepare in accordance with the following steps:
Weigh the lithium carbonate of certain chemical ratios, nickel protoxide, (this chemical ratios is known ratio to Red copper oxide, at this slightly Go), adopt water as grinding aid, zirconium oxide is ball-milling medium, and ratio of grinding media to material is 5:1, and solid content is 60%, utilizes nanometer to grind high-speed stirring Mixing, obtaining granularity D50 is the homogeneous mixture about 3 μm.Have another name called by the metering score of 1:0.5:1.5 and take Lithium hydrate, nitric acid Nickel, manganese nitrate are dissolved in alcohol solvent, then make it to colloidal sol shape with ammonia regulation PH, obtain nickel ion doped colloidal sol.By 2% Nickel ion doped colloidal sol, D50 are that the mangano-manganic oxide of 12 μm joins in aforesaid homogeneous mixture, open nanometer and grind and open and follow Ring pump, stirring at low speed 1h, 90 DEG C are dynamically dried.By first for the mixture after dry combustion method high-temperature calcination 12h at a temperature of 950 DEG C, then Anneal at a temperature of 710 DEG C 24h, i.e. obtains required big particle diameter spinel-type nickel ion doped LiNi0.45Mn1.45Cu0.1O4.By gained Material for electric performance test, 0.2C specific discharge capacity is 136mAh/g, and room temperature 1C 200 weeks capability retentions of circulation are 99% Above, 200 weeks capability retentions of high temperature 1C circulation are more than 93%.
Embodiment 6:
A kind of big particle diameter spinel-type nickel ion doped LiNi0.5Mn1.45Zn0.05O4Synthesis, prepare in accordance with the following steps:
Weigh the lithium carbonate of certain chemical ratios, nickel protoxide, zinc oxide (this chemical ratios is known ratio, omits) at this, Adopting water as grinding aid, zirconium oxide is ball-milling medium, and ratio of grinding media to material is 9:1, and solid content is 65%, utilizes nanometer to grind high-speed stirred, It is the homogeneous mixture about 5 μm to granularity D50.Have another name called by the metering score of 1:0.5:1.5 and take Lithium hydrate, nickel nitrate, nitre Acid manganese is dissolved in alcohol solvent, then makes it to colloidal sol shape with ammonia regulation PH, obtains nickel ion doped colloidal sol.By the nickel manganese of 13% Acid lithium colloidal sol, D50 are that the mangano-manganic oxide of 15 μm joins in aforesaid homogeneous mixture, open nanometer mill ON cycle Pump, stirring at low speed 1h, 100 DEG C are dynamically dried.By first for the mixture after dry combustion method high-temperature calcination 12h at a temperature of 910 DEG C, then Anneal at a temperature of 710 DEG C 18h, i.e. obtains required big particle diameter spinel-type nickel ion doped LiNi0.5Mn1.45Zn0.05O4.By gained Material for electric performance test, 0.2C specific discharge capacity is 132mAh/g, and room temperature 1C 200 weeks capability retentions of circulation are 98% Above, 200 weeks capability retentions of high temperature 1C circulation are more than 91%.

Claims (9)

1. the preparation method of a big particle diameter spinel-type nickel ion doped, it is characterised in that comprise the steps:
(1) high speed ball milling after the compound of Li, Ni and doped chemical M being mixed with certain chemical ratios, it is thus achieved that Li, Ni, M's Homogeneous mixture A；
(2) lithium salts, nickel salt, manganese salt being dissolved in alcohol solvent according to the chemical ratios of 1:0.5:1.5, ammonia is adjusted to colloidal sol shape, Obtain nickel ion doped sol B；
(3) the homogeneous mixture A of Li, Ni, M, nickel ion doped sol B and Mn oxide C mix and blend are mixed, be dried to obtain mixed Compound D；
(4) mixture D high temperature sintering is obtained nickel ion doped material.
The preparation method of a kind of big particle diameter spinel-type nickel ion doped the most according to claim 1, it is characterised in that: described Step (1) in, the compound of Li, Ni, M is oxide, carbonate, nitrate, acetate, oxalates or hydroxide In the mixture of one or more.
The preparation method of a kind of big particle diameter spinel-type nickel ion doped the most according to claim 1, it is characterised in that: described Step (1) in, doped chemical M is nickel position or Mn-site doping, and be Al, Co, Cr, Zn, Y, Fe, Ag, Ca, V, Cu, Zr, Ti, One or both elements in Sn, Mo, La, Ce, Pr, Nd.
The preparation method of a kind of big particle diameter spinel-type nickel ion doped the most according to claim 1, it is characterised in that: described Step (1) in, the particle size range of homogeneous mixture A is 100nm～5 μm.
The preparation method of a kind of big particle diameter spinel-type nickel ion doped the most according to claim 1, it is characterised in that: described Step (2) in, lithium salts, nickel salt, manganese salt are the one in nitrate, acetate, oxalates, carbonate or hydroxide or many The mixture planted.
The preparation method of a kind of big particle diameter spinel-type nickel ion doped the most according to claim 1, it is characterised in that: described Step (3) in, add nickel ion doped sol B ratio be 1%～20%.
The preparation method of a kind of big particle diameter spinel-type nickel ion doped the most according to claim 1, it is characterised in that: described Step (3) in, Mn oxide C is particle diameter manganese dioxide in 5～15 μ m or mangano-manganic oxide.
The preparation method of a kind of big particle diameter spinel-type nickel ion doped the most according to claim 1, it is characterised in that: described Step (3) in, the mixture of homogeneous mixture A, nickel ion doped sol B and Mn oxide C be dried be 70～100 DEG C dynamically It is dried.
The preparation method of a kind of big particle diameter spinel-type nickel ion doped the most according to claim 3, it is characterised in that: described Ratio a of doped chemical M is in the range of 0 ＜ a≤0.5m, and wherein, m is the ratio of institute's substitute element position.
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CN109437340A (en) * 2018-12-07 2019-03-08 长安大学 A kind of rare earth modified NiMn2O4Spinel powder and its preparation method and application
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CN113517437A (en) * 2021-07-14 2021-10-19 中国石油大学(北京) Cation modified spinel type lithium nickel manganese oxide and preparation method and application thereof

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