CN1316652C - Cobalt acid lithium battery material adulterated alkaline-earth metal between layers and its preparing method - Google Patents

Cobalt acid lithium battery material adulterated alkaline-earth metal between layers and its preparing method Download PDF

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CN1316652C
CN1316652C CNB2004100864664A CN200410086466A CN1316652C CN 1316652 C CN1316652 C CN 1316652C CN B2004100864664 A CNB2004100864664 A CN B2004100864664A CN 200410086466 A CN200410086466 A CN 200410086466A CN 1316652 C CN1316652 C CN 1316652C
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earth metal
cobalt acid
lithium
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alkaline
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杨文胜
段雪
李秀梅
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Beijing University of Chemical Technology
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Abstract

The present invention relates to a novel interlaminar doping cobalt acid lithium anode material which is doped by alkaline earth metal ions instead of lithium ions and a preparation method thereof for fused salt ion exchange reaction. The chemical composition of the anode material is Li<1-2 beta> (AE) beta CoO2 (AE=Mg, Ca). The preparation method has the steps that a laminar cobalt acid lithium LiCoO2 precursor body with small and uniform particle diameter is prepared by a citric acid sol-gel method; some lithium ions in the laminar cobalt acid lithium is replaced by the alkaline earth metal ions Mg (2+) or Ca (2+) through the fused salt ion exchange reaction; the lithium ions and the alkaline earth metal ions are uniformly distributed on an interlayer of a main body plywood made of CoO2 by a baking and homogenizing process; the interlaminar doping cobalt acid lithium is obtained. When the cobalt acid lithium anode material is in the process of charge and discharge cycle, the lithium ions Li (+) can be reversibly separated from inlay, but the alkaline earth metal ions Mg (2+) and Ca (2+) can not be separated so as to play the function of stable support on the plywood interlayer and keep the lamellar structure characteristics of the electrode material. Thereby, the interlaminar doping cobalt acid lithium electrode material has the advantages of stable structure, better anti-overcharge performance, higher specific capacity and finer electrochemical cycle performance in the process of the charge and discharge cycle.

Description

Cobalt acid lithium battery material of a kind of adulterated alkaline-earth metal between layers and preparation method thereof
Technical field
The present invention relates to cobalt acid lithium battery material of a kind of adulterated alkaline-earth metal between layers and preparation method thereof, belong to lithium ion battery material and preparing technical field thereof.
Background technology
Has α-NaFeO 2The LiCoO of type layer structure 2Having excellent electrochemical properties the most in present various anode material for lithium-ion batteries, is the main positive electrode of commercialization lithium ion battery.But LiCoO 2Cost an arm and a leg actual specific capacity 120～140mAhg -1, only be its theoretical capacity (274mAhg -1) about 50%; LiCoO 2The anti-over-charging electrical property relatively poor, specific capacity reduces rapidly under higher charging voltage.For overcoming LiCoO 2The problem that exists, multiple modified measures and method have been taked in people's research.
It is to adopt Ni that present people study more method of modifying, Al, and Ti, multiple element such as Fe carries out doped and substituted to Co, in the hope of reaching the purpose of stabilizing material structure.As at document (1) Solid State Ionics, 2003, among the 159:241, people such as Chi-Hwan Han have synthesized Part of Co Al, the LiCo that Ni replaces 0.8M 0.2O 2(M=Al, Ni) compound, wherein LiCo 0.8Ni 0.2O 2Discharge capacity first reach 146 mAh/g, 20 times circulation back capacity still remains on 130mAh/g.Many elements in the periodic table of elements have been used to the doped and substituted of Co, but except that the doped and substituted of only a few element (as Ni etc.) can not cause the reduction of reversible specific capacity first, the doped and substituted of other elements all can make its first reversible specific capacity reduce significantly, and the doped and substituted of elements such as Ni does not have obvious effect for the anti-over-charging electrical property that improves material.
Another important modification means are at LiCoO 2The surface coats Al 2O 3, P 2O 5, ALPO 4, materials such as MgO improve the pernicious interaction between electrode material and electrolyte, the dissolving that slows down cobalt.As at document (2) SolidState Ionics, 2002, among the 148:335, people such as Zhaoxiang Wang are at LiCoO 2The surface has coated MgO, Al 2O 3, SnO 2Deng metal oxide, wherein the product of MgO coating is 4.7V (vs.Li when charging by voltage +/ still have good electrochemistry cycle performance Li) time.But metal oxides such as MgO all are the non-electrochemical active material, it adds the reduction that affiliation causes the electrode material reversible capacity, in addition, therefore the method does not change the body construction of material, is that the raising of electrochemistry cycle performance and anti-over-charging performance there is no remarkable effect to the structural stability of electrode material.
Summary of the invention
Stratiform LiCoO 2In charging process, with laminate interlayer Li +Constantly deviating from of ion, the repulsive force between the main body laminate strengthens, and the laminate spacing is constantly expanded, and when the laminate spacing increased to a certain degree (promptly overcharging), laminate subsided, and irreversible transition takes place, and made LiCoO 2Electrochemical specific capacity reduce rapidly.Purpose of the present invention is exactly in order to solve stratiform LiCoO 2This problem that exists provides the lithium cobaltate cathode material and the fused salt ion-exchange reactions preparation method thereof of the novel adulterated alkaline-earth metal between layers of a kind of lithium ion battery.
The lithium cobaltate cathode material of adulterated alkaline-earth metal between layers provided by the invention is with the part lithium ion Li in the stratiform cobalt acid lithium +Use alkaline-earth metal ions Mg 2+Or Ca 2+Replace.Its chemical composition general formula is Li 1-2 β(A E) βCoO 2, A in the formula EA kind of among alkali earth metal Mg, the Ca, and 0.02≤β≤0.05; Cobalt and oxygen constitute CoO with covalent bonds 2Main body laminate, lithium ion and alkaline-earth metal ions are positioned at body layer plate holder layer, combine with ionic bond with electronegative main body laminate, have typical α-NaFeO 2The type layer structure belongs to hexagonal crystal system,
Figure C20041008646600051
Space group.
This lithium cobaltate cathode material in the charge and discharge cycles process, lithium ion Li +Can reversiblely take off embedding, and alkaline-earth metal ions Mg 2+, Ca 2+Can not deviate from, play the stable support effect at the laminate interlayer, the layer structure feature that keeps electrode material, so the cobalt of adulterated alkaline-earth metal between layers acid lithium electrode material has more in the charge and discharge cycles process, and stable structure, better anti-over-charging electrical property, higher specific capacity reach better electrochemistry cycle performance.
The lithium cobaltate cathode material of this adulterated alkaline-earth metal between layers adopts fused salt ion-exchange reactions method to prepare.Promptly adopt earlier the citric acid sol-gel process prepare particle diameter tiny all-stratiform cobalt acid lithium LiCoO 2Presoma passes through the fused salt ion-exchange reactions then with the part lithium ion Li in the stratiform cobalt acid lithium +Use alkaline-earth metal ions Mg 2+Or Ca2 +Replace, by the roasting homogeneous lithium ion and alkaline-earth metal ions are evenly distributed on by CoO again 2The interlayer of the main body laminate that constitutes obtains interlayer doping cobalt acid lithium Li thus 1-2 βA E βCoO 2(A E=Mg, Ca).
Concrete processing step is as follows:
A is the mixed of 1.05～1.15/1/2.05～2.15 with lithium hydroxide, basic cobaltous carbonate and citric acid by Li/Co/ citric acid mol ratio, is dissolved in the deionized water, is made into Li +Concentration be 2～4molL -1Solution, in Rotary Evaporators, under the condition of 50～80 ℃ of temperature, 40～100rpm rotating speed, react 2～3h, form peony colloidal sol, be transferred to then in the vacuum drying chamber,, obtain fluffy red xerogel in 100～140 ℃ of vacuumize 3～4h, xerogel is obtained the floccule of pitchy at 400～500 ℃ of preliminary treatment 2～5h, be reentered into after the grinding in the Muffle furnace,, obtain meeting the LiCoO of stoichiometric proportion and the tiny homogeneous of particle diameter in 800～900 ℃ of following roasting 3～9h 2Product.
The stratiform cobalt acid lithium presoma that B obtains steps A is 1/5～1/15 mixed according to mol ratio with having low-melting alkaline earth metal compound, carry out the fused salt ion-exchange reactions being higher than under 20～50 ℃ of temperature of alkaline earth metal compound fusing point, the reaction time is 10min～300min.
Used low-melting alkaline earth metal compound that has is: magnesium nitrate hexahydrate Mg (NO 3) 26H 2O (89 ℃ of fusing points), magnesium chloride hexahydrate MgCl 26H 2O (116 ℃ of fusing points), calcium chloride hexahydrate CaCl 26H 2O (29.9 ℃ of fusing points), four water-calcium nitrate Ca (NO 3) 24H 2A kind of among the O (42.7 ℃ of fusing points).
C with ion exchange product with aprotic solvent flush away alkaline earth metal compound more than needed, in vacuum drying chamber with vacuumize 2～3h under 70～100 ℃ the temperature.Used aprotic solvent is: acetone CH 3COCH 3, carbon tetrachloride CCl 4, cyclohexane C 6H 12In a kind of.
D with step C gained material with 2～10 ℃ of min -1Speed is warming up to 300～500 ℃ and constant temperature 5～20h, naturally cools to room temperature then, obtains product of the present invention.
Adopt day island proper Tianjin ICPS-7500 type inductive coupling plasma emission spectrograph to measure the content of lithium, alkaline-earth metal and cobalt in the product, day island proper Tianjin XRD-6000 type x-ray powder diffraction instrument (CuK αRadiation, λ=1.5406 ) characterize product structure, the Mastersizer of Britain Ma Erwen company 2000 type laser particle size analyzers are measured the particle diameter and the distribution of product.Test result shows: adopt the citric acid sol-gel process to prepare and meet LiCoO 2The stratiform cobalt of stoichiometric proportion acid lithium presoma, the chemical composition of the product that obtains by fused salt ion-exchange reactions method is Li 1-2 βA E βCoO 2(A E=Mg, Ca); Presoma and ion-exchange afterproduct all belong to hexagonal crystal system, and have good crystal formation; Cobalt acid lithium presoma and the tiny homogeneous of ion-exchange afterproduct particle diameter, particle size distribution range 0.8～1.2 μ m, integrable cloth 1.0 μ m.
Respectively embodiment 1,2 and 3 synthetic electrode materials and commercially available acetylene black conductive agent and the polytetrafluoroethylene binding agent mass fraction by 85: 10: 5 is mixed, and the thickness of compressing tablet to 100 μ m, in 120 ℃ of vacuum (＜1Pa) dry 24h.As to electrode, adopt Celgard 2400 barrier films, 1molL with metal lithium sheet -1LiPF 6+ EC+DMC (EC/DMC volume ratio 1: 1) is an electrolyte, at the German M. Braun Unlab of company type dry argon gas glove box (H 2O＜1ppm, O 2＜be assembled into Experimental cell in 1ppm), adopt the blue electric BTI1-10 type cell tester in Wuhan to carry out electrochemical property test, the results are shown in Table 1.Comparative sample adopts the synthetic stratiform cobalt acid lithium LiCoO of citric acid sol-gel process for the present invention 2Presoma.Also contrast the Electrochemical results of having listed the sample with higher chemical property of report in the document 1,2 in the table 1.
The electrochemistry cycle performance of table 1 electrode material
Sample Chemical composition Test condition Reversible capacity mAhg -1
First 10 20 30
Embodiment 1 Li 0.95Ca 0.025CoO 2 3.0～4.3V，0.2mA·cm -2 152 149 147 146
3.0～4.5V，0.2mA·cm -2 177 173 170 168
3.0～4.7V，0.2mA·cm -2 211 196 192 189
Embodiment 2 Li 0.90Ca 0.05CoO 2 3.0～4.5V，0.2mA·cm -2 175 170 166 164
3.0～4.7V，0.2mA·cm -2 209 203 198 194
Embodiment 3 Li 0.95Mg 0.025CoO 2 3.0～4.5V，0.2mA·cm -2 178 174 171 170
3.0～4.7V，0.2mA·cm -2 213 198 194 191
Comparative sample LiCoO 2 3.0～4.3V，0.2mA·cm -2 147 144 142 140
3.0～4.5V，0.2mA·cm -2 178 166 154 145
3.0～4.7V，0.2mA·cm -2 210 171
Document (1) LiCoO 2 2.8～4.3V，70mA·g -1 139 122
LiCo 0.8Ni 0.2O 2 2.8～4.3V，70mA·g -1 146 132
Document (2) LiCoO 2 2.5～4.5V，0.1mA·cm -2 190 80
2.5～4.7V，0.1mA·cm -2 265 100
MgO-LiCoO 2 2.5～4.5V，0.1 mA·cm -2 170 160
2.5～4.7V，0.1mA·cm -2 210 195
Remarkable result of the present invention as can be seen from Table 1 is: compare with adopting other element dopings replacement Co and surface coated method of modifying, the interlayer doping cobalt acid lithium of the inventive method preparation can not cause the reduction of initial capacity, and has stable structure more, better anti-over-charging electrical property, higher specific capacity and better electrochemistry cycle performance.
Embodiment
Embodiment 1:
With lithium hydroxide, basic cobaltous carbonate and citric acid is raw material, takes by weighing raw material and mixes in the ratio of Li/Co/ citric acid=1.1/1/2.1 (mol ratio), is dissolved in the deionized water, is made into Li +Concentration be 4molL -1Solution, (75 ℃, 60rpm) reaction 2h in Rotary Evaporators, form peony colloidal sol, be transferred to then in the vacuum drying chamber, in 120 ℃ of vacuumize 3h, obtain fluffy red xerogel, xerogel at the floccule that 500 ℃ of preliminary treatment 3h obtain pitchy, after the grinding, is reentered in the Muffle furnace, in 850 ℃ of following roasting 6h, obtain meeting the LiCoO of stoichiometric proportion 2Product is as the presoma of fused salt ion-exchange reactions.
With four water-calcium nitrate Ca (NO 3) 24H 2O and stratiform LiCoO 2Presoma is pressed the mixed of Ca/Li=5 (mol ratio), heating and continuous stirring reaction 2h in 70 ℃ of water-baths, and decompress filter and with acetone washing three times, filter cake at 500 ℃ of roasting 10h, obtains product again at 70 ℃ of vacuumize 3h.ICP and XRD test shows product consist of Li 0.95Ca 0.025CoO 2, belonging to hexagonal crystal system, Electrochemical results sees Table 1.
Embodiment 2:
With lithium hydroxide, basic cobaltous carbonate and citric acid is raw material, takes by weighing raw material and mixes in the ratio of Li/Co/ citric acid=1.15/1/2.15 (mol ratio), is dissolved in the deionized water, is made into Li +Concentration be the solution of 3molL-1, (80 ℃, 60rpm) reaction 3h in Rotary Evaporators, form peony colloidal sol, be transferred to then in the vacuum drying chamber, in 140 ℃ of vacuumize 3h, obtain fluffy red xerogel, xerogel at the floccule that 450 ℃ of preliminary treatment 3h obtain pitchy, after the grinding, is reentered in the Muffle furnace, in 900 ℃ of following roasting 6h, obtain meeting the LiCoO of stoichiometric proportion 2Product is as the presoma of fused salt ion-exchange reactions.
With calcium chloride hexahydrate CaCl 26H 2O and stratiform LiCoO 2Presoma is pressed the mixed of Ca/Li=5 (mol ratio), heating and continuous stirring reaction 4h in 60 ℃ of water-baths, and decompress filter and with cyclohexane washing three times, filter cake at 450 ℃ of roasting 15h, obtains product again at 80 ℃ of vacuumize 2h.ICP and XRD test shows product consist of Li 0.9Ca 0.05CoO 2, belonging to hexagonal crystal system, Electrochemical results sees Table 1.
Embodiment 3:
Adopt with embodiment 1 same procedure and prepare stratiform LiCoO 2Presoma.
With magnesium nitrate hexahydrate Mg (NO 3) 26H 2O and stratiform LiCoO 2Presoma takes by weighing raw material and mixing in the ratio of Mg/Li=15 (mol ratio), heating and continuous stirring reaction 4h in 120 ℃ of oil baths, decompress filter and with acetone washing three times, filter cake is at 90 ℃ of vacuumize 3h, again at 400 ℃ of roasting 15h, obtain product of the present invention, ICP and XRD test shows product consist of Li 0.95Mg 0.025CoO 2, belonging to hexagonal crystal system, Electrochemical results sees Table 1.

Claims (2)

  1. The cobalt acid lithium battery material of 1 one kinds of adulterated alkaline-earth metal between layers, chemical composition general formula are Li 1-2 β(A E) βCoO 2, A in the formula EA kind of among alkali earth metal Mg, the Ca, and 0.02≤β≤0.05; Cobalt and oxygen constitute CoO with covalent bonds 2Main body laminate, lithium ion and alkaline-earth metal ions are positioned at body layer plate holder layer, combine with ionic bond with electronegative main body laminate, have typical α-NaFeO 2The type layer structure belongs to hexagonal crystal system,
    Figure C2004100864660002C1
    Space group.
  2. The preparation method of the cobalt acid lithium battery material of 2 one kinds of adulterated alkaline-earth metal between layers as claimed in claim 1, processing step is as follows:
    A is the mixed of 1.05～1.15/1/2.05～2.15 with lithium hydroxide, basic cobaltous carbonate and citric acid by Li/Co/ citric acid mol ratio, is dissolved in the deionized water, is made into Li +Concentration be 2～4molL -1Solution, in Rotary Evaporators, under the condition of 50～80 ℃ of temperature, 40～100rpm rotating speed, react 2～3h, form peony colloidal sol, be transferred to then in the vacuum drying chamber,, obtain fluffy red xerogel in 100～140 ℃ of vacuumize 3～4h, xerogel is obtained the floccule of pitchy at 400～500 ℃ of preliminary treatment 2～5h, be reentered into after the grinding in the Muffle furnace,, obtain meeting the LiCoO of stoichiometric proportion and the tiny homogeneous of particle diameter in 800～900 ℃ of following roasting 3～9h 2Product;
    The LiCoO that B obtains steps A 2Is 1/5～1/15 mixed with having low-melting alkaline earth metal compound according to mol ratio, carries out the fused salt ion-exchange reactions under than high 20～50 ℃ temperature of the fusing point of alkaline earth metal compound, and the reaction time is 10min～300min;
    Described alkaline earth metal compound is: Mg (NO 3) 26H 2O, MgCl 26H 2O, CaCl 26H 2O, Ca (NO 3) 24H 2A kind of among the O;
    C with ion exchange product with aprotic solvent flush away alkaline earth metal compound more than needed, in vacuum drying chamber with temperature vacuumize 2～3h of 70～100 ℃;
    Described aprotic solvent is: a kind of in acetone, carbon tetrachloride, the cyclohexane;
    D with step C gained material with 2～1O ℃ of min -1Speed is warming up to 300～500 ℃ and constant temperature 5～20h, naturally cools to room temperature then, obtains product;
    The chemical composition general formula of this product is Li 1-2 β(A E) βCoO 2, A in the formula EA kind of among alkali earth metal Mg, the Ca, and 0.02≤β≤0.05; Cobalt and oxygen constitute CoO with covalent bonds 2Main body laminate, lithium ion and alkaline-earth metal ions are positioned at body layer plate holder layer, combine with ionic bond with electronegative main body laminate, have typical α-NaFeO 2The type layer structure belongs to hexagonal crystal system, Space group.
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CN104332599B (en) * 2014-11-13 2016-06-15 湖南杉杉能源科技股份有限公司 The preparation method of a kind of lithium cobalt oxide solid solution presoma
KR102147364B1 (en) 2016-12-21 2020-08-24 주식회사 엘지화학 Metal Doped-Positive Active Material for High Voltage
CN109314238B (en) * 2016-12-21 2022-04-01 株式会社Lg化学 Metal-doped positive electrode active material for high voltage
CN109786738B (en) * 2017-11-15 2021-02-12 华为技术有限公司 High-voltage lithium cobalt oxide cathode material, preparation method thereof and lithium ion battery
KR102389411B1 (en) 2017-12-08 2022-04-22 주식회사 엘지에너지솔루션 Lithium cobalt based positive electrode active material, producing method thereof, positive electrode and secondary battery comprising the same
CN110797511A (en) * 2018-08-01 2020-02-14 华为技术有限公司 Lithium ion battery positive electrode material and preparation method and application thereof
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