CN1847155A - Prepn process of polynary positive pole material of lithium ion cell with compound transition metal oxide as intermediate product - Google Patents

Prepn process of polynary positive pole material of lithium ion cell with compound transition metal oxide as intermediate product Download PDF

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CN1847155A
CN1847155A CNA2006100247832A CN200610024783A CN1847155A CN 1847155 A CN1847155 A CN 1847155A CN A2006100247832 A CNA2006100247832 A CN A2006100247832A CN 200610024783 A CN200610024783 A CN 200610024783A CN 1847155 A CN1847155 A CN 1847155A
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lithium
intermediate product
positive pole
transition metal
metal oxide
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CN100372774C (en
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夏保佳
张建
韩学武
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Shanghai Institute of Microsystem and Information Technology of CAS
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Abstract

The present invention relates to the preparation process of polynary positive pole material of lithium ion cell. The polynary positive pole material is prepared through first preparation of compound transition metal oxide in spinel structure as the intermediate product, the subsequent mixing with lithium salt and final high temperature calcining. The polynary positive pole material has composition of LiNixCoyMn(1-x-y)O2, where, x is 0.1-0.8, y is 0.1-0.5, and x+y is 0.5-1.0. The polynary positive pole material has homogeneous granularity distribution, specific discharge capacity in 2.8-4.3 V/Li up to 157 mAh/g, excellent circulating stability and low cost, and is suitable for use in lithium ion cell.

Description

Compound transition metal oxide prepares the method for polynary positive pole material of lithium ion cell as intermediate product
Technical field
The present invention relates to a kind of lithium ion battery preparation method, or rather, relate in order to compound transition metal oxide as intermediate product by relating to the method that the solid phase calcination legal system is equipped with the polynary positive pole material of lithium ion cell of excellent property with polynary positive pole material.Belong to the lithium ion battery electrode material field.
Technical background
Along with mobile electron consuming product such as mobile phone, digital camera, notebook computer, PDA and hand-held camera continue become popular and lithium-ion-power cell presents huge application potential, the market requirement of following lithium ion battery will keep suitable rate of growth.The annual requirement of the traditional positive pole material of lithium cobalt acid in the whole world surpasses 10,000 tons, thereby causes the cobalt valency unprecedented soaring, and inadequate resource has begun to restrict industry development.The poor heat stability of the lithium of cobalt acid simultaneously.When lithium ion cell charging is above to 4.2V, it easily reacts with electrolytic solution and causes the battery temperature rising, cause cobalt acid lithium decomposition and emit very big heat, inner pressure of battery increases simultaneously, finally may cause battery explosion, thereby safety performance is relatively poor, and this has limited the application of lithium ion battery as power cell.Therefore, the equivalent material of exploitation cobalt acid lithium is significant to lithium ion battery development from now on.Studies show that the most over the past two years, polynary positive pole material LiNi xCo yMn 1-x-yO 2Compare with cobalt acid lithium, have the specific storage height, security reaches advantages such as cost is low well, be widely regarded as can be practical anode material for lithium-ion batteries, the research of its synthetic method is paid close attention to by various countries, wherein more representative have: codeposition synthesis method, promptly earlier synthetic Ni xCo yMn 1-x-y(OH) 2Or Ni xCo yMn 1-x-yCO 3Presoma is mixed in proportion presoma and lithium salts again, obtains LiNi through high temperature sintering xCo yMn 1-x-yO 2Solid phase method mixes lithium salts by a certain percentage with the salt or the oxide compound of transition metal, and high-temperature calcination forms again.
Through discovering, though product structure homogeneous, even particle size distribution and chemical property that method makes are good, it is single-phase that this method requires the presoma of preparation and size distribution is even, just can make the finished product have desired good performance.Need the condition of strict control co-precipitation when synthesizing presoma, this is difficult in actually operating, and this method synthesis procedure complexity needs the equipment of usefulness also many simultaneously, and the production cycle is long in the reality operation, investment is big, is unfavorable for industrialization.Method is 2. simple to operate, production efficiency is high, but solid state reaction mainly relies on the diffusion between the material in the sintering process, the slow and unavoidable ununiformity of physical mixed because of diffusion, make that finishing entire reaction course needs higher temperature and long time, and there is bigger difference in product inside at aspects such as composition, structure and granularities, cause the chemical property of product wayward, poor reproducibility is difficult to realize industrialization.
Summary of the invention
The objective of the invention is to overcome the shortcoming of existing synthetic method, a kind of polynary positive pole material of lithium ion cell of being prepared excellent property by compound transition metal oxide as intermediate product is provided.
It is starting raw material that the present invention selects transistion metal compound and lithium salts for use, by preparing compound transition metal oxide as intermediate product, mixes after high-temperature calcination forms with lithium salts more earlier, and it comprises the steps:
(1) preparation of compound transition metal oxide intermediate product
1. according to positive electrode material LiNi xCo yMn 1-x-yO 2Composition take by weighing the compound thorough mixing of nickel (Ni), cobalt (Co), manganese (Mn).The nickel of selecting for use, cobalt, manganic compound comprise one or more in the material groups such as oxide compound, oxyhydroxide, carbonate, nitrate or acetate.
2. with said mixture high-temperature calcination a few hours in air, obtain Ni, Co, the Mn ternary compound oxides of spinel structure, wherein calcining temperature 500-900 ℃, soaking time 2-15 hour.
(2) polynary positive pole material of lithium ion cell is synthetic
3. after above-mentioned composite oxides being mixed as intermediate product and lithium salts, high-temperature calcination a few hours in air.The lithium salts of selecting for use comprises in the material groups such as Quilonum Retard, lithium hydroxide, lithium nitrate, Lithium Acetate at least two kinds; Promptly two or three.
4. cool off, pulverize above-mentioned calcining materials;
5. with the calcining materials pulverized high-temperature calcination a few hours once more in air;
6. cool off, pulverize, sieve that promptly to obtain chemical formula be LiNi xCo yMn 1-x-yO 2Polynary positive pole material of lithium ion cell.
Wherein reaction conditions is: step calcining temperature 500-800 3. ℃, and time 2-20 hour; 5. third firing temperature of step 700-1000 ℃, time 3-30 hour.
The nickel of step described in 1., cobalt, manganic compound mix and add organic solvent wet mixings such as water or ethanol earlier, do after the oven dry again and mix, and it is mixed.
The compound transition metal oxide intermediate product of step described in 3. mixes organic solvent wet mixings such as adding water or ethanol earlier with lithium salts, do after the oven dry again and mix, and it is mixed; Polynary positive pole material of lithium ion cell consists of LiNi xCo yMn 1-x-yO 2(wherein 0.1≤x≤0.8,0.1≤y≤0.5,0.5≤x+y＜1.0).
Wet mixing time, the amount of using solvent and bake out temperature etc. are that those skilled in the art are familiar with, wet mixing, driedly do time unsuitable longly or too short, and the long production cycle prolongs, and the loss meeting of abrading-ball increases, and be too short obviously inhomogeneously mixed.And the wet mixing time was advisable with 0.5-2 hour, was advisable in the dried 0.5-5 of doing time hour.
The present invention compares with existing method, has the following advantages:
1, prepares compound transition metal oxide earlier as intermediate product, join lithium again and calcine.Because these composite oxides are Ni, Co, the Mn ternary homogeneous oxidizing thing of spinel structure, have guaranteed that final product has stable chemical constitution and structure.The composite oxide particle size that obtains through high-temperature calcination is big, density is high, helps improving the density of final product, and then promotes the energy density of lithium ion battery.
2, select for use multiple lithium salts as the lithium source, rather than single lithium source, may be because the synergy that the different decomposition characteristic of different lithium salts, reactive behavior and potential of hydrogen produce promote the fully reaction of lithium and composite oxides ground, so final product has excellent electrochemical properties;
3, present method technology is simple, and the technology of step (2) is similar to the high temperature solid phase synthesis of the lithium of very sophisticated cobalt acid, can play reference function, helps realizing industrialization.And the positive electrode material of the present invention's preparation has the identical performance of material (seeing embodiment 1 for details is comparative example 2) of coprecipitate complicated technology preparation.
Description of drawings
Fig. 1: the XRD figure spectrum of the composite oxides intermediate product of the spinel structure of the embodiment of the invention;
Fig. 2: the LiNi of the embodiment of the invention 1 0.5Co 0.2Mn 0.3O 2XRD figure spectrum;
Fig. 3: the LiNi of the embodiment of the invention 1 0.5Co 0.2Mn 0.3O 2The SEM photo;
Fig. 4: the LiNi of the embodiment of the invention 1 0.5Co 0.2Mn 0.3O 2The charging and discharging curve second time (0.5C, 2.8～4.3V) of/Li button cell; X-coordinate is a capacity, and unit is mAh/g; Ordinate zou is a voltage, and unit is V;
Fig. 5: the LiNi of the embodiment of the invention 0.5Co 0.2Mn 0.3O 2The cyclic curve of/Li button cell (0.5C, 2.8～4.3V); X-coordinate is a cycle index; Ordinate zou is a capacity, and unit is mAh/g.
Embodiment
Below in conjunction with specific embodiment method for preparing multielement cathode materials for lithium ion batteries of the present invention is described further.
Embodiment 1
With synthetic LiNi 0.5Co 0.2Mn 0.3O 2Be example, metering takes by weighing the oxide compound (mol ratio of Ni: Co: Mn=5: 2: 3) of nickel, cobalt, manganese, added the water wet mixing 1 hour, oven dry is done and was mixed 3 hours after mixing, and fully stirring makes and mixes, change over to and carry out the first step calcining in the sintering oven, 800 ℃ of calcining temperatures, soaking time 6 hours promptly obtains the compound transition metal oxide intermediate product, compose as can be seen from the XRD figure of Fig. 1, this intermediate product is the single-phase composite oxides of spinel structure.
By metering lithium hydroxide and lithium nitrate (mol ratio of lithium hydroxide and lithium nitrate is 1: 1) are added the composite oxides intermediate product, elder generation's wet mixing is done and is mixed (method is the same), carry out the calcining of second step behind the thorough mixing, calcining temperature is 600 ℃ in the air, soaking time 8 hours.Carry out the calcining of the 3rd step, 900 ℃ of calcining temperatures, soaking time 20 hours after cooling, the pulverizing.Cooling is after ball milling promptly obtains final product LiNi 0.5Co 0.2Mn 0.3O 2Compose as can be seen the LiNi of preparation from the XRD figure of Fig. 2 0.5Co 0.2Mn 0.3O 2Material is α-NaFeO 2Single-phase laminate structure.Scheme as can be seen the LiNi of preparation from the SEM of Fig. 3 0.5Co 0.2Mn 0.3O 2Material is the class sphere, and size-grade distribution is more even.Be positive active material with the lithium sheet with this material be that counter electrode is assembled into button cell and carries out electrochemical property test, the discharge curve of battery such as Fig. 4.The polynary positive pole material of lithium ion cell specific discharge capacity height that the present invention is prepared reaches 157mAh/g, and the capability retention that circulates after 50 times is 86%.
The comparative example 1
Adopt the synthetic LiNi of solid phase method 0.5Co 0.2Mn 0.3O 2, the oxide compound of nickel, cobalt, manganese and Quilonum Retard are mixed the back do and mix, through 600 ℃ of pyroprocessing 8 hours.Calcined 20 hours down at 900 ℃ cooling, pulverizing back.Cooling is after ball milling obtains final product LiNi 0.5Co 0.2Mn 0.3O 2This material is at 0.5C, and the specific discharge capacity under 2.8～4.3V/Li condition is 148mAh/g, and the capability retention that circulates after 50 times is 70%.
The comparative example 2
Adopt co-electrodeposition method to prepare Ni earlier 0.5Co 0.2Mn 0.3(OH) 2Presoma, with presoma with after lithium hydroxide mixes, through 500 ℃ of pyroprocessing 8 hours.Calcined 20 hours down at 900 ℃ cooling, pulverizing back.Cooling is after ball milling obtains final product LiNi 0.5Co 0.2Mn 0.3O 2This material is at 0.5C, and the specific discharge capacity under 2.8～4.3V/Li condition is 158mAh/g, and the capability retention that circulates after 50 times is 88%.
By present embodiment and Comparative Examples as seen, the positive electrode material of compatible composition adopts method preparation provided by the invention, and its performance obviously is better than solid phase method synthetic material, and compares with existing coprecipitation method, performance is approaching, thereby further embodies substantive distinguishing features of the present invention and obvious improvement.
Embodiment 2
Metering takes by weighing nickel hydroxide, Xiao Suangu and manganous carbonate (mol ratio of Ni: Co: Mn=3: 3: 3), and (hybrid mode is with embodiment 1) calcines after mixing, 900 ℃ of calcining temperatures, and soaking time 4 hours obtains compound transition metal oxide.By metering Quilonum Retard and Lithium Acetate (mol ratio of Quilonum Retard and Lithium Acetate is 2: 1) are added the composite oxides intermediate product, mix back (hybrid mode is with embodiment 1),, be incubated 5 hours through 700 ℃.Again through 950 ℃, calcined 10 hours after cooling, the pulverizing.Cooling is after ball milling promptly obtains final product LiNi 1/3Co 1/3Mn 1/3O 2This material is at 0.5C, and the specific discharge capacity under 2.8～4.3V/Li condition is 151mAh/g, and the capability retention that circulates after 50 times is 92%.
Embodiment 3
Metering takes by weighing nickelous nitrate, Cobaltous diacetate and Manganse Dioxide (mol ratio of Ni: Co: Mn=7: 2: 1), uses the ethanol wet mixing earlier, does after the oven dry again and mixes, calcine afterwards, and 500 ℃ of calcining temperatures, soaking time 15 hours obtains compound transition metal oxide.By metering Quilonum Retard, lithium hydroxide and lithium nitrate (mol ratio of Quilonum Retard, lithium hydroxide and lithium nitrate is 1: 1: 1) are added the composite oxides intermediate product, mix back (hybrid mode is with embodiment 1),, be incubated 15 hours through 500 ℃.Again through 800 ℃, calcined 30 hours after cooling, the pulverizing.Cooling is after ball milling promptly obtains final product LiNi 0.7Co 0.2Mn 0.1O 2This material is at 0.5C, and the specific discharge capacity under 2.8～4.3V/Li condition is 154mAh/g, and the capability retention that circulates after 50 times is 83%.
Polynary positive pole material of lithium ion cell LiNi xCo yMn 1-x-yO 2The consumption of middle cobalt reduces greatly, the specific storage height, and good cycling stability can replace cobalt acid lithium and be used for lithium ion battery.The polynary positive pole material of lithium ion cell that the present invention is prepared as intermediate product by compound transition metal oxide is better than the material of general solid phase method preparation on performance, can with the material of co-electrodeposition method preparation shoulder to shoulder, to be higher than co-electrodeposition method aspect the density of positive electrode material.Therefore, preparation method's thinking novelty of the present invention, excellent property, characteristics are remarkable, have actual application value.

Claims (10)

1. one kind prepares the method for polynary positive pole material of lithium ion cell with compound transition metal oxide as intermediate product, described positive electrode material consist of LiNi xCO yMn 1-x-yO 2, 0.1≤x in the formula≤0.8,0.1≤y≤0.5,0.5≤x+y＜1.0, it is characterized in that selecting the compound of transition metal Ni, Co and Mn and lithium salts for use is starting raw material, earlier the preparation compound transition metal oxide is as intermediate product, mixes with lithium salts to form through high-temperature calcination again.
2. prepare the method for polynary positive pole material of lithium ion cell with compound transition metal oxide as intermediate product by claim 1 is described, it is characterized in that comprising the steps:
(1) preparation of compound transition metal oxide intermediate product
1. according to positive electrode material LiNi xCo yMn 1-x-yO 2Composition take by weighing the compound of nickel, cobalt, manganese;
2. with said mixture 500-900 ℃ of calcining in air, soaking time 2-15 hour, obtain Ni, Co, the Mn ternary compound oxides of spinel structure;
(2) polynary positive pole material of lithium ion cell is synthetic
3. after the composite oxides that 2. step is prepared mix as intermediate product and lithium salts, high-temperature calcination a few hours in air.
4. cool off, pulverize above-mentioned calcining materials;
5. with the calcining materials pulverized high-temperature calcination for the third time a few hours in air;
6. cool off, pulverize, sieve that promptly to obtain chemical formula be LiNi xCo yMn 1-x-yO 2Polynary positive pole material of lithium ion cell;
Wherein reaction conditions is: step calcining temperature 500-800 3. ℃, and time 2-20 hour; 5. third firing temperature of step 700-1000 ℃, time 3-30 hour.
3. describedly prepare the method for polynary positive pole material of lithium ion cell with compound transition metal oxide as intermediate product by claim 1 or 2, wherein said nickel, cobalt, manganic compound are one or more in oxide compound, oxyhydroxide, carbonate, nitrate or the acetate.
4. prepare the method for polynary positive pole material of lithium ion cell with compound transition metal oxide as intermediate product by claim 1 is described, wherein said lithium salts is in Quilonum Retard, lithium hydroxide, lithium nitrate and the Lithium Acetate at least two kinds.
5. by the described method for preparing polynary positive pole material of lithium ion cell with compound transition metal oxide as intermediate product of claim 2, the mixing that it is characterized in that the compound of nickel during step 1., cobalt, manganese is to add water or ethanol wet mixing earlier, do again after the oven dry and mix, the wet mixing time is 0.5-2 hour, and dried doing time is 0.5-5 hour.
6. by the described method for preparing polynary positive pole material of lithium ion cell with compound transition metal oxide as intermediate product of claim 2, it is characterized in that multiple platform oxide compound is to add water or ethanol wet mixing earlier as intermediate product and lithium salts uniform mixing during step 3., do again after the oven dry and mix, the wet mixing time is 0.5-2 hour, and dried doing time is 0.5-5 hour.
7. prepare the method for polynary positive pole material of lithium ion cell with compound transition metal oxide as intermediate product by claim 4 is described, it is characterized in that employed lithium salts is lithium hydroxide and lithium nitrate, both mol ratios are 1: 1.
8. prepare the method for polynary positive pole material of lithium ion cell with compound transition metal oxide as intermediate product by claim 4 is described, it is characterized in that employed lithium salts is Quilonum Retard, lithium hydroxide and lithium nitrate, three's mol ratio is 1: 1: 1.
9. prepare the method for polynary positive pole material of lithium ion cell with compound transition metal oxide as intermediate product by claim 4 is described, it is characterized in that employed lithium salts is lithium nitrate and Lithium Acetate, both mol ratios are 2: 1.
10. describedly prepare the method for polynary positive pole material of lithium ion cell as intermediate product by claim 1 or 2, it is characterized in that prepared LiNi with compound transition metal oxide 0.5Co 0.2Mn 0.3O 2Material is α-NaFeO 2Single-phase laminate structure, and be the class sphere.
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