CN103647074A - High-rate type lithium cobaltate and preparation method thereof - Google Patents
High-rate type lithium cobaltate and preparation method thereof Download PDFInfo
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- CN103647074A CN103647074A CN201310740089.0A CN201310740089A CN103647074A CN 103647074 A CN103647074 A CN 103647074A CN 201310740089 A CN201310740089 A CN 201310740089A CN 103647074 A CN103647074 A CN 103647074A
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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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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
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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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Abstract
The invention discloses a preparation method of high-rate type lithium cobaltate, and relates to a process method of the high-rate lithium cobaltate, which belongs to the novel energy resource material technology. The preparation method comprises the following steps: firstly, adding a cobalt material and doped substances (oxides or organic substances of Mg, Al, Ti, Zr, Nb, and the like) in proportion and uniformly dispersing in an organic dispersing solvent, adding lithium carbonate for mixing, sintering for 8 hours-20 hours after drying at a high temperature of 900DEG C-1000 DEG C under an atmosphere condition of 100m<3>/hour-200m<3>/hour; and then, carrying out pulverization treatment by a high-speed rotary device to obtain the lithium cobaltate with good rate capability. The method disclosed by the invention is simple, convenient to implement, excellent in product rate capability and low in processing cost.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries field, relate generally to a kind of high magnification type cobalt acid lithium and preparation method thereof.
Background technology
Since lithium ion battery commercialization, because its operating voltage is high, energy density is large, long service life, operating temperature range are wide, memory-less effect and the advantage such as pollution-free, in communication, has moved with the field such as electric tool and be used widely rapidly.Along with the continuous expansion of range of application, to the requirement of lithium ion battery also in continuous renewal.As fields such as the car mould of present rise, model plane, ship model, electronic cigarette, electric automobiles, now also bring into use lithium ion battery as power resources.These commodity need to meet its use needs by lasting high current charge-discharge, so the lithium ion battery of rate also constantly upgrades and tries out.
Use cobalt acid lithium as the positive active material of rate battery, subject matter is the control of particle size and crystal morphology.When particle diameter becomes large, under high-multiplying power discharge, discharging efficiency step-down, when particle diameter diminishes, poor processability, security performance and cycle performance also can decrease.
Summary of the invention
The present invention is in order to solve the problems of the technologies described above, a kind of high magnification type cobalt acid lithium and preparation method thereof is provided, the high magnification cobalt acid lithium material that obtains modification by controlling cobalt acid lithium primary particle size and crystal morphology, the method is simple, the large-scale industrial production that is applicable to low cost.
The present invention is achieved through the following technical solutions:
A preparation method for high magnification type cobalt acid lithium, comprises the following steps:
(1) in organic dispersion solvent, by the mol ratio of Y/Co 0.005～0.02, add oxide and the cobalt oxide raw material of Y, form mixed liquor, wherein Y is at least one in Mg, Al, Ti, Zr, Nb element; By above-mentioned mixed liquor in liquid dispersion equipment with 1000-15000rpm high speed dispersion 5-20min, the mixed liquor after being disperseed;
(2) by Li/Co mol ratio, be to re-use the dry 1-3h of vacuum dryer after adding lithium carbonate to mix in the mixed liquor of 1.00-1.05 after above-mentioned dispersion, obtain dried mixture;
(3) by step 2) in the mixture that obtains at 900-1000 ℃, air atmosphere 100-200m
3sintering 8-20h under the condition of/h;
(4) use high-speed rotating equipment under 800-1500rpm condition, to carry out broken pulverization process 5-40min in the mixture after sintering, control average grain diameter (D50) in 2-7um, obtain high magnification type cobalt acid lithium.
Cobalt oxide raw material in described step (1) is spherical cobalt oxide raw material, and average grain diameter (D50) is 2-6um.
Described spherical cobalt oxide raw material, average grain diameter (D50) is 3.5-5.5um.
The organic dispersion solvent using in described step (1) is ethanol, acetone.
By above-mentioned mixed liquor in liquid dispersion equipment with 2000rpm high speed dispersion 5-20min, the mixed liquor after being disperseed.
In described step (2), Li/Co mol ratio is 1.00-1.03.
The mixture just obtaining in step (2) is at 940-970 ℃, air atmosphere 145-200m
3sintering 8-20h under the condition of/h.
Use high-speed rotating equipment under 1000-1300rpm condition, to carry out broken pulverization process 5-10min in the mixture after sintering, control average grain diameter (D50) in 2-7um, obtain high magnification type cobalt acid lithium.
Described liquid dispersion equipment is mulser, sand mill.
A kind of high magnification type cobalt acid lithium powder of being prepared by the preparation method of high magnification type cobalt acid lithium, primary granule particle diameter of this cobalt acid lithium powder is between 1-3um, the secondary behavior grain diameter (D50) that primary particle is agglomerated into is between 2-7um, and this cobalt acid lithium powder meets chemical formula Li
1+xco
1-yy
yo
2, wherein, Y is one or more in Mg, Al, Ti, Zr, Nb, 0.01≤x≤0.10; 0.005≤y≤0.02.
Compared with prior art, the present invention has following useful technique effect:
High magnification type cobalt acid lithium provided by the invention and preparation method thereof, after being added in proportion, cobalt oxide raw material and dopant (oxide or the organic substances of Mg, Al, Ti, Zr, Nb etc.) be uniformly dispersed in organic dispersion soln, add again lithium raw material to mix, dry after at high temperature and the 100-200m of 900-1000 ℃
3sintering 8-20h under the atmospheric condition of/h, is then used that high-speed dispersion equipment carries out obtaining after powdered processing that particle size is suitable, the cobalt acid lithium of crystal morphology and good rate capability.This method technique is simple, and it is convenient to implement, the outstanding and low processing cost of product high rate performance.
Cobalt prepared by the present invention acid lithium powder is at discharge-rate under the heavy-current discharge condition at 35C, 40C, 45C, 50C, capacity can reach 1C discharge capacity 95.5%, 94.5%, 94%, more than 93%.
Accompanying drawing explanation
The Electronic Speculum figure that Fig. 1 is the high magnification type cobalt acid lithium powder manufactured by embodiment 2;
The Electronic Speculum figure that Fig. 2 is the high magnification type cobalt acid lithium powder manufactured by embodiment 3;
The Electronic Speculum figure that Fig. 3 is the high magnification type cobalt acid lithium powder manufactured by comparative example 1;
Fig. 4 is the XRD figure of high magnification type cobalt acid lithium provided by the invention.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
Embodiment 1, and a kind of preparation method of high magnification type cobalt acid lithium, comprises the following steps:
(1) in organic dispersion solvent, by the mol ratio of Y/Co 0.005～0.02, add oxide and the cobalt oxide raw material of Y, form mixed liquor, wherein Y is at least one in the elements such as Mg, Al, Ti, Zr, Nb; By above-mentioned mixed liquor in liquid dispersion equipment with 1000-15000rpm high speed dispersion 5-20min, the mixed liquor after being disperseed.The organic dispersion solvent using in described step (1) is ethanol, acetone.
Preferably, the cobalt oxide raw material in described step (1) is spherical cobalt oxide raw material, and average grain diameter (D50), in 2-6um, is preferably in 3.5-5.5um.
By above-mentioned mixed liquor in liquid dispersion equipment with 2000rpm high speed dispersion 5-20min, the equipment that can fully disperse the powder in liquid, the mixed liquor after being disperseed.Described liquid dispersion equipment is mulser, sand mill.
(2) by Li/Co mol ratio, be to re-use the dry 1-3h of vacuum dryer after adding lithium carbonate to mix in the mixed liquor of 1.00-1.05 after above-mentioned dispersion, obtain dried mixture.In preferred described step (2), Li/Co mol ratio is 1.00-1.03.
(3) by step 2) in the mixture that obtains sintering 8-20 hour under 900-1000 ℃, the condition of air atmosphere 100-200m3/h.Preferably, by step 2) in the mixture that obtains sintering 8-20h under 940-970 ℃, the condition of air atmosphere 145-200m3/h.
(4) use high-speed rotating equipment under 800-1500rpm condition, to carry out broken pulverization process 5-40min in the mixture after sintering, control average grain diameter (D50) in 2-7um, obtain high magnification type cobalt acid lithium.
Preferably, use high-speed rotating equipment under 1000-1300rpm condition, to carry out broken pulverization process 5-10min in the mixture after sintering, control average grain diameter (D50) in 2-7um, obtain high magnification type cobalt acid lithium.
Referring to Fig. 1, Fig. 4, embodiment 2, and a kind of preparation method of high magnification cobalt acid lithium, comprises following steps:
(1) in the sand mill of 300L, add the ethanol of about 200L as dispersant, the ratio that is 0.01 in Ti/Co ratio adds TiO
2and cobalt oxide, stir 20min.
(2) under the condition that is 1.01 by the mol ratio of Li/Co, add lithium carbonate in sand mill, to mix 10 minutes, re-use vacuum dryer dry 2 hours.
(3) will obtain mixture at 950 ℃, pass into air atmosphere 145m
3under/h condition, constant temperature sintering 14h.
(4) sinter is used high-speed rotating equipment under 1200rpm condition, carry out broken pulverization process 8min, obtain average grain diameter (D50) for 5.73um.
By prepared cobalt acid lithium and acetylene black, PVDF in mass ratio 94:3:3 add appropriate NMP to mix, be coated on aluminium foil.In vacuum drying oven, at 105 ℃, toast after 10h, take out and carry out compressing tablet, cut-parts.Take cobalt acid lithium as anodal, and graphite pole piece is negative pole, and electrolyte adopts 1M LiPF
6-EC/DMC(volume ratio is 1:1), in being full of the glove box of argon gas, assemble full battery, battery size is 803496.And use battery performance test instrument to carry out electric performance test to battery.Discharging and recharging cut-ff voltage is 3～4.2V, rate of charge is 0.2C, recording 1C specific discharge capacity is first 155.1mAh/g, and the discharge capacity under different discharge-rate 35C, 40C, 45C, 50C reaches respectively 96.8%, 95.5%, 95.3%, 94.6% of 1C discharge capacity.
Referring to Fig. 2, Fig. 4, embodiment 3: a kind of preparation method of high magnification cobalt acid lithium, comprises following steps:
(1) in the sand mill of 300L, add the ethanol of about 200L as dispersant, the ratio that is 0.01 in Zr/Co ratio adds ZrO
2and cobalt oxide, stir 20 minutes.
(2) under the condition that is 1.01 by the mol ratio of Li/Co, add lithium carbonate in sand mill, to mix 10 minutes, re-use the dry 2h of vacuum dryer.
(3) will obtain mixture at 950 ℃, pass into air atmosphere 145m
3under/h condition, constant temperature sintering 14h.
(4) sinter is used high-speed rotating equipment under 1200rpm condition, carry out broken pulverization process 8min, obtain average grain diameter (D50) for 5.73um.
By prepared cobalt acid lithium and acetylene black, PVDF in mass ratio 94:3:3 add appropriate NMP to mix, be coated on aluminium foil.In vacuum drying oven, at 105 ℃, toast after 10h, take out and carry out compressing tablet, cut-parts.Take cobalt acid lithium as anodal, and graphite pole piece is negative pole, and electrolyte adopts 1M LiPF
6-EC/DMC(volume ratio is 1:1), in being full of the glove box of argon gas, assemble full battery, battery size is 803496.And use battery performance test instrument to carry out electric performance test to battery.Discharging and recharging cut-ff voltage is 3～4.2V, rate of charge is 0.2C, recording 1C specific discharge capacity is first 155.1mAh/g, and the discharge capacity under different discharge-rate 35C, 40C, 45C, 50C reaches respectively 95.8%, 94.7%, 94.3%, 94.1% of 1C discharge capacity.
Embodiment 4: a kind of preparation method of high magnification cobalt acid lithium, comprises following steps:
(1) in the sand mill of 300L, add the ethanol of about 200L as dispersant, the ratio that is 0.02 in Mg/Co ratio adds MgO and cobalt oxide, stirs 12.5min.
(2) under the condition that is 1.05 by the mol ratio of Li/Co, add lithium carbonate in sand mill, to mix 10min, re-use the dry 1h of vacuum dryer.
(3) will obtain mixture at 1000 ℃, pass into air atmosphere 100m
3under/h condition, constant temperature sintering 8h.
(4) sinter is used high-speed rotating equipment under 800rpm condition, carry out broken pulverization process 40min, obtain average grain diameter (D50) for 4.5um.
Embodiment 5: a kind of preparation method of high magnification cobalt acid lithium, comprises following steps:
(1) in the sand mill of 300L, add the ethanol of about 200L as dispersant, the ratio that is 0.005 in Al/Co ratio adds Al
2o
3and cobalt oxide, stir 5min.
(2) under the condition that is 1.025 by the mol ratio of Li/Co, add lithium carbonate in sand mill, to mix 10min, re-use the dry 3h of vacuum dryer.
(3) will obtain mixture at 900 ℃, pass into air atmosphere 200m
3under/h condition, constant temperature sintering 20h.
(4) sinter is used high-speed rotating equipment under 1500rpm condition, carry out broken pulverization process 5min, obtain average grain diameter (D50) for 7um.
Referring to Fig. 3, comparative example 1:
With embodiment 1, except only having lithium and cobalt raw material in step (1), temperature makes 1010 ℃ into, and atmospheric condition is at 80m
3under/h condition, carry out.The discharge capacity of the cobalt acid lithium material obtaining under different discharge-rate 35C, 40C, 45C, 50C is respectively 80.2%, 75.3%, 72.8%, 69.9% of 1C discharge capacity.
Referring to Fig. 1 to Fig. 4, a kind of high magnification type cobalt acid lithium powder of preparing according to the preparation method of high magnification type cobalt acid lithium, primary granule particle diameter of this cobalt acid lithium powder is between 1-3um, the secondary behavior grain diameter (D50) that primary particle is agglomerated into is between 2-7um, and this cobalt acid lithium powder meets chemical formula Li
1+xco
1-yy
yo
2, wherein, Y is one or more in Mg, Al, Ti, Zr, Nb, 0.01≤x≤0.10; 0.005≤y≤0.02.
The present invention makes cobalt acid lithium powder at discharge-rate under the heavy-current discharge condition at 35C, 40C, 45C, 50C, capacity can reach 1C discharge capacity 95.5%, 94.5%, 94%, more than 93%.
The present invention obtains the high magnification cobalt acid lithium material of modification by controlling product primary particle size and crystal morphology, to be applied to high-power power consumption equipment, as model plane etc.The method is simple, the large-scale industrial production that is applicable to low cost.
More than show and described basic principle of the present invention and principal character and advantage of the present invention.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (10)
1. a preparation method for high magnification type cobalt acid lithium, is characterized in that, comprises the following steps:
(1) in organic dispersion solvent, by the mol ratio of Y/Co 0.005～0.02, add oxide and the cobalt oxide raw material of Y, form mixed liquor, wherein Y is at least one in Mg, Al, Ti, Zr, Nb element; By above-mentioned mixed liquor in liquid dispersion equipment with 1000-15000rpm high speed dispersion 5-20min, the mixed liquor after being disperseed;
(2) by Li/Co mol ratio, be to re-use the dry 1-3h of vacuum dryer after adding lithium carbonate to mix in the mixed liquor of 1.00-1.05 after above-mentioned dispersion, obtain dried mixture;
(3) by the mixture obtaining in step (2) sintering 8-20h under 900-1000 ℃, the condition of air atmosphere 100-200m3/h;
(4) use high-speed rotating equipment under 800-1500rpm condition, to carry out broken pulverization process 5-40min in the mixture after sintering, control average grain diameter (D50) in 2-7um, obtain high magnification type cobalt acid lithium.
2. the preparation method of high magnification type cobalt acid lithium according to claim 1, is characterized in that, the cobalt oxide raw material in described step (1) is spherical cobalt oxide raw material, and average grain diameter (D50) is 2-6um.
3. the preparation method of high magnification type cobalt acid lithium according to claim 2, is characterized in that, described spherical cobalt oxide raw material, and average grain diameter (D50) is 3.5-5.5um.
4. the preparation method of high magnification type cobalt acid lithium according to claim 1, is characterized in that, the organic dispersion solvent using in described step (1) is ethanol, acetone.
5. the preparation method of high magnification type cobalt according to claim 1 acid lithium, is characterized in that, by above-mentioned mixed liquor in liquid dispersion equipment with 2000rpm high speed dispersion 5-20min, the mixed liquor after being disperseed.
6. the preparation method of high magnification type cobalt acid lithium according to claim 1, is characterized in that, in described step (2), Li/Co mol ratio is 1.00-1.03.
7. the preparation method of high magnification type cobalt according to claim 1 acid lithium, is characterized in that, just step 2) in the mixture that obtains at 940-970 ℃, air atmosphere 145-200m
3sintering 8-20h under the condition of/h.
8. the preparation method of high magnification type cobalt according to claim 1 acid lithium, it is characterized in that, use high-speed rotating equipment under 1000-1300rpm condition, to carry out broken pulverization process 5-10min in the mixture after sintering, control average grain diameter (D50) in 2-7um, obtain high magnification type cobalt acid lithium.
9. the preparation method of high magnification type cobalt acid lithium according to claim 1, is characterized in that, described liquid dispersion equipment is mulser, sand mill.
10. high magnification type cobalt that according to claim 1 prepared by a method acid lithium powder, it is characterized in that, primary granule particle diameter of this cobalt acid lithium powder is between 1-3um, and the secondary behavior grain diameter (D50) that primary particle is agglomerated into is between 2-7um, and this cobalt acid lithium powder meets chemical formula Li
1+xco
1-yy
yo
2, wherein, Y is one or more in Mg, Al, Ti, Zr, Nb, 0.01≤x≤0.10; 0.005≤y≤0.02.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104009230A (en) * | 2014-05-30 | 2014-08-27 | 深圳市巨兆数码有限公司 | Lithium ion battery anode material and lithium ion battery |
| CN104157830A (en) * | 2014-07-06 | 2014-11-19 | 魏斌 | Novel LiCo(1-x)AlxO2 electrode material and preparation method thereof |
| CN106486665A (en) * | 2016-11-01 | 2017-03-08 | 北大先行科技产业有限公司 | A kind of low internal resistance lithium cobaltate cathode material and its preparation method and application |
| CN111370689A (en) * | 2020-03-16 | 2020-07-03 | 电子科技大学 | Ruthenium and aluminum co-doped lithium cobalt oxide positive electrode material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005071623A (en) * | 2003-08-21 | 2005-03-17 | Seimi Chem Co Ltd | Producing method for lithium cobalt composite oxide for secondary battery positive electrode |
| CN102779976A (en) * | 2011-10-10 | 2012-11-14 | 北大先行科技产业有限公司 | Preparation method of cathode material of LCO (lithium cobaltate)-based lithium ion battery |
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- 2013-12-25 CN CN201310740089.0A patent/CN103647074B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005071623A (en) * | 2003-08-21 | 2005-03-17 | Seimi Chem Co Ltd | Producing method for lithium cobalt composite oxide for secondary battery positive electrode |
| CN102779976A (en) * | 2011-10-10 | 2012-11-14 | 北大先行科技产业有限公司 | Preparation method of cathode material of LCO (lithium cobaltate)-based lithium ion battery |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104009230A (en) * | 2014-05-30 | 2014-08-27 | 深圳市巨兆数码有限公司 | Lithium ion battery anode material and lithium ion battery |
| CN104157830A (en) * | 2014-07-06 | 2014-11-19 | 魏斌 | Novel LiCo(1-x)AlxO2 electrode material and preparation method thereof |
| CN106486665A (en) * | 2016-11-01 | 2017-03-08 | 北大先行科技产业有限公司 | A kind of low internal resistance lithium cobaltate cathode material and its preparation method and application |
| CN111370689A (en) * | 2020-03-16 | 2020-07-03 | 电子科技大学 | Ruthenium and aluminum co-doped lithium cobalt oxide positive electrode material and preparation method thereof |
| CN111370689B (en) * | 2020-03-16 | 2022-05-03 | 电子科技大学 | Ruthenium and aluminum co-doped lithium cobalt oxide positive electrode material and preparation method thereof |
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