CN102544506B - Method for preparing lithium battery anode material - Google Patents
Method for preparing lithium battery anode material Download PDFInfo
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- CN102544506B CN102544506B CN201110434737.0A CN201110434737A CN102544506B CN 102544506 B CN102544506 B CN 102544506B CN 201110434737 A CN201110434737 A CN 201110434737A CN 102544506 B CN102544506 B CN 102544506B
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- lithium
- dry
- battery anode
- anode material
- lithium battery
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
Abstract
The invention relates to a lithium battery anode material and a method for preparing the lithium battery anode material, belonging to the field of the method for preparing the battery anode material. The method comprises the following steps: adding an improver into lithium-nickel-cobalt-manganese oxide precursor solution or lithium-nickel-cobalt-manganese oxide based doped precursor solution, carrying out chemical reaction at low temperature to prepare lithium-nickel-cobalt-manganese oxide or lithium-nickel-cobalt-manganese oxide based doped material, and sintering a synthetic product which is used as the lithium battery anode. The process for preparing the lithium battery anode material has a considerable margin and is easy to control. The product can be mixed uniformly in the molecular level, and the energy consumed in the process for preparing the lithium battery anode material can be reduced. The specific capacity and the cycling stability of the 3C electronic product battery are improved, and the safety factor and the environmental-protection factor are considered. The application of the lithium battery anode material to the fields of electronic products and energy can be expanded.
Description
Technical field
The present invention relates to a kind of positive electrode and method of battery, particularly a kind of method preparing anode material of lithium battery.
Background technology
Development clean energy resource is the task of top priority of the modern life, and the generation modes such as solar energy, wind energy, tide are very unstable, all need obtained energy storage.Nuclear energy power generation is reliable and stable but the level radioactive nuclear waste of association must reprocessing.Though geother-mal power generation cleans but is limited to region, not have everywhere.In addition energy storage mainly relies on electric energy at present, and this comprises electrical network, electromagnetic wave, chemical energy storage etc.The easiest mode, surely belongs to portable chemical energy storage device battery, and it effectively can change chemical energy into electric energy and without waste gas generation, and the easy chemical energy that transferred to by electric energy stores again.
Graphite has the advantages such as capacity is high, inexpensive, safe as lithium cell cathode material, and the key that therefore lithium battery develops at present is to improve further capacity, the fail safe of positive electrode and reduces costs.Conventional anode material of lithium battery has LiCoO
2, LiMn
2o
4, LiFePO
4and LiNi
1/3co
1/3mn
1/3o
2deng, wherein LiMn
2o
4and LiFePO
4be suitable for electrokinetic cell, LiCoO
2and LiNi
1/3co
1/3mn
1/3o
2then be more suitable for 3C electronic product.
The preparation method of positive electrode is divided into pure solid-phase sintering, wet method making precursor to combine calcining, hydro thermal method etc. again.Material has its shortcoming with the manufacture of pure solid phase method sintering traditionally, such as high temperature, long-time, the difficult metering obtaining fixing component are than, the composition not easily undesirable element such as too wide, the easy introducing impurity of Homogeneous phase mixing, particle size distribution, make end product undesirable, affect battery performance; If use Moist chemical synthesis presoma instead again in conjunction with sintering, then can improve above shortcoming.And can energy consumption be reduced, expand its range of application.The cell positive material of multiple wet-layer preparation lithium nickel cobalt manganese oxygen is disclosed in existing document and technology, need to adjust pH pH-value when the cell positive material described in preparing, manufacture process is comparatively loaded down with trivial details, or uses stronger acidity, alkaline environment to follow-up environmental protection treatment, will increase burden.
Summary of the invention
the object of the invention is to provide a kind of method preparing anode material of lithium battery, it is undesirable that during solution dry fabrication cell positive material, temperature is high, the time grows final active material, affects battery performance; During wet method, need to adjust pH pH-value, acid, alkaline to the disadvantageous problem of environmental protection.
The object of the present invention is achieved like this: the preparation method of cell positive material is in the precursor solution of lithium nickel cobalt manganese oxygen or the doping type oxide that is matrix with it, add improver respectively, undertaken by chemical reaction at low temperatures, the doping type material preparing lithium nickel cobalt manganese oxygen or be matrix with it, then calcines the positive pole that synthetic product is used for lithium battery.Concrete preparation method is:
After stoichiometrically taking nickel acetate, cobalt acetate and manganese acetate, add appropriate amount of deionized water and be mixed with the mixed solution that metal cation adds up to 0.1 M.Prepare the lithium hydroxide mixed solution of 0.2 M, and add 0.01M ethanol/isopropyl alcohol, ethanol and isopropanol ratios are 1:1.Control mixing speed, dropwise mixed-cation solution is added drop-wise in lithium hydroxide solution.After ageing 24 h, cyclic washing is centrifugal for several times, then dry obtained presoma in drying box.To be dried complete after, grinding is evenly; Then stoichiometrically, namely excessive 5 wt.% take lithium source lithium hydroxide, after mixing with presoma, and compressing tablet on powder compressing machine; 26 h are sintered at 900 DEG C, obtained target product Li in resistance furnace
1.09ni
0.29co
0.145mn
0.47o
2, stand-by after grinding; With powder x-ray diffraction, X-ray diffraction analysis is carried out to product;
Product in mass ratio: PVDF: after carbon black=85:8:7 takes each material, dry 12 h at 80 DEG C in vacuum drying chamber; The N-methyl measuring respective volume in the ratio of 1 g PVDF: 25 ml NMP adjoins pyrrolidone NMP, then with Kynoar PVDF mix and blend; After PVDF is fully swelling, active material and carbon black are joined in this solution, continue to stir, until it mixes; Then after evenly smear is approximately 16 mm aluminium flakes to diameter, dry in baking oven; Treat that positive plate is fully dry, compressing tablet, then dry 12 h at vacuum drying chamber 120 DEG C after removal NMP, put into glove box again and prepare assembling test after weighing; Described NMP is that N-methyl adjoins pyrrolidone; Described PVDF is Kynoar;
Being assemblied in the glove box being full of argon gas of battery is carried out, and in the pre-assembly, is cleaned up by button cell shell with acetone, to remove the greasy dirt on surface, and dry 24 h; Assembly operation step is: place button cell cathode shell and lithium sheet successively, then drip electrolyte 1 M LiPF
6eC/DEC ratio be 1:1 on lithium sheet, place Celgard 2400 barrier film, then drip electrolyte on barrier film, finally place positive plate and anode cover; Seal on button cell sealing instrument, after placing 24 h hours, carry out the test of battery capacity performance; Carry out capacity test at 2-4.8V with 0.05C current density, specific discharge capacity reaches 200 mAh/g.
Described lithium nickel cobalt manganese oxygen presoma, adopts the one in the hydroxide of each element of lithium nickel cobalt manganese, acetate, nitrate, carbonate.
The base and doped type compound of described lithium nickel cobalt manganese oxygen, be divided into cation doping and anion doped two kinds, wherein cation doping is Zn
2+, Cu
2+, Fe
3+, Sn
4+, Ta
5+, Nb
5+in one or more, anion doped is F
-, Cl
-, S
2-, N
3-, C
4-in one or more.
preparation process of the present invention has suitable nargin, easily controls, and makes product reach other Homogeneous phase mixing of molecular level, is minimized the energy consumption in preparation process.And for improving specific capacity, the stable circulation performance of 3C electronic product battery, taking into account the factor such as safety and environmental protection, being beneficial to and expanding its application at electronic product and energy field.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) collection of illustrative plates of the embodiment of the present invention 1.
Fig. 2 is the charging and discharging curve of the embodiment of the present invention 1.
Fig. 3 is the cycle performance figure of the embodiment of the present invention 2.
Embodiment
Below by embodiment in detail the present invention is described in detail.
Embodiment 1:
After stoichiometrically taking nickel acetate, cobalt acetate and manganese acetate, add appropriate amount of deionized water and be mixed with the mixed solution that metal cation adds up to 0.1 M.Prepare the lithium hydroxide mixed solution of 0.2 M, and add 0.01M ethanol/isopropyl alcohol, ethanol and isopropanol ratios are 1:1.Control mixing speed, dropwise mixed-cation solution is added drop-wise in lithium hydroxide solution.After ageing 24 h, cyclic washing is centrifugal for several times, then dry obtained presoma in drying box.To be dried complete after, grinding is evenly.Then stoichiometrically (excessive 5 wt.%) take lithium source lithium hydroxide, after mixing with presoma, and compressing tablet on powder compressing machine.26 h are sintered at 900 DEG C, obtained target product Li in resistance furnace
1.09ni
0.29co
0.145mn
0.47o
2, stand-by after grinding.Carry out X-ray diffraction analysis with powder x-ray diffraction (Rigaku Dmax3B, Cu K α) to product, its result as shown in Figure 1, can be found out well-crystallized in figure, there is not impurity peaks, illustrates that purity is high.
Product in mass ratio: PVDF: after carbon black=85:8:7 takes each material, dry 12 h at 80 DEG C in vacuum drying chamber.The N-methyl measuring respective volume in the ratio of 1 g PVDF: 25 ml NMP adjoins pyrrolidone (NMP), then with Kynoar (PVDF) mix and blend.After PVDF is fully swelling, active material and carbon black are joined in this solution, continue to stir, until it mixes.Then after evenly smear is approximately 16 mm aluminium flakes to diameter, dry in baking oven.Until positive plate fully dry (removing NMP) afterwards compressing tablet, then dry 12 h at vacuum drying chamber 120 DEG C, put into glove box after weighing again and prepare assembling test.
Being assemblied in the glove box being full of argon gas of battery is carried out, and in the pre-assembly, is cleaned up by button cell shell with acetone, to remove the greasy dirt on surface, and dry 24 h.Assembly operation step is: place button cell cathode shell and lithium sheet successively, then drip electrolyte 1 M LiPF
6eC/DEC (1:1) on lithium sheet, place Celgard 2400 barrier film, then drip electrolyte on barrier film, finally place positive plate and anode cover.Seal on button cell sealing instrument, after placing 24 h hours, carry out the test of battery capacity performance.Carry out capacity test at 2-4.8V with 0.05C current density, as shown in Figure 2, specific discharge capacity reaches 200 mAh/g to charge-discharge test curve, illustrates functional.
Embodiment 2:
After stoichiometrically taking nickel chloride, cobalt acetate and manganese sulfate, add appropriate amount of deionized water and be mixed with the mixed solution that metal cation adds up to 0.1 M.Prepare the NaOH mixed solution of 0.2 M, and add 0.01M ethanol/isopropyl alcohol, ethanol and isopropanol ratios are 1:1, control mixing speed, are dropwise added drop-wise in lithium hydroxide solution by mixed-cation solution.After ageing 20 h, cyclic washing is centrifugal for several times, then dry obtained presoma in drying box.To be dried complete after, grinding is evenly.Then stoichiometrically (excessive 5 wt.%) take lithium source lithium carbonate, after mixing with presoma, and compressing tablet on powder compressing machine.In resistance furnace, sinter 4 h at 400 DEG C, at 900 DEG C, sinter 22 h, obtained target product Li
1.167ni
0.2co
0.1mn
0.53o
2, through the test as embodiment 1, specific discharge capacity 200 mAh/g can be obtained.
Embodiment 3:
After stoichiometrically taking nickel chloride, cobalt chloride, zinc sulfate and manganese acetate, add appropriate amount of deionized water and be mixed with the mixed solution that metal cation adds up to 0.1 M.Prepare the NaOH mixed solution of 0.2 M, and add 0.01M ethanol.Control mixing speed, dropwise mixed-cation solution is added drop-wise in lithium hydroxide solution.After ageing 20 h, cyclic washing is centrifugal for several times, then dry obtained presoma in drying box.To be dried complete after, grinding is evenly.Then stoichiometrically (excessive 5 wt.%) take lithium source lithium hydroxide, after mixing with presoma, and compressing tablet on powder compressing machine.In resistance furnace, sinter 2 h at 450 DEG C, at 800 DEG C, sinter 30 h, obtained target product Li
1.167ni
0.18co
0.98zn
0.04mn
0.53o
2, through the test as embodiment 1, specific discharge capacity 200 mAh/g can be obtained.
Embodiment 4:
After stoichiometrically taking nickelous sulfate, cobalt acetate, zirconium dioxide and manganese chloride, add appropriate amount of deionized water and be mixed with the mixed solution that metal cation adds up to 0.1 M.Prepare the NaOH mixed solution of 0.2 M, and add 0.01M ethanol.Control mixing speed, dropwise mixed-cation solution is added drop-wise in lithium hydroxide solution.After ageing 20 h, cyclic washing is centrifugal for several times, then dry obtained presoma in drying box.To be dried complete after, grinding is evenly.Then stoichiometrically (excessive 5 wt.%) take lithium source lithium carbonate, after mixing with presoma, and compressing tablet on powder compressing machine.In resistance furnace, sinter 4 h at 350 DEG C, at 780 DEG C, sinter 40 h, obtained target product Li
1.13ni
0.22co
0.13mn
0.45zr
0.06o
2, through the test as embodiment 1, specific discharge capacity 200 mAh/g can be obtained.
Embodiment 5:
After stoichiometrically taking nickel nitrate, cobalt nitrate, copper sulphate and manganese nitrate, add appropriate amount of deionized water and be mixed with the mixed solution that metal cation adds up to 0.1 M.Prepare the NaOH mixed solution of 0.2 M, and add 0.01M ethanol/isopropyl alcohol, ethanol and isopropanol ratios are 1:1.Control mixing speed, dropwise mixed-cation solution is added drop-wise in lithium hydroxide solution.After ageing 20 h, cyclic washing is centrifugal for several times, then dry obtained presoma in drying box.To be dried complete after, grinding is evenly.Then stoichiometrically (excessive 5 wt.%) take lithium source lithium hydroxide, after mixing with presoma, and compressing tablet on powder compressing machine.In resistance furnace, sinter 4 h at 350 DEG C, at 850 DEG C, sinter 30 h, obtained target product Li
1.13ni
0.23co
0.13mn
0.45cu
0.05o
2, through the test as embodiment 1, specific discharge capacity 200 mAh/g can be obtained.
Embodiment 6:
After stoichiometrically taking nickel nitrate, cobalt nitrate, aluminium hydroxide and manganese nitrate, add appropriate amount of deionized water and be mixed with the mixed solution that metal cation adds up to 0.1 M.Prepare the NaOH mixed solution of 0.2 M, and add 0.01M isopropyl alcohol.Control mixing speed, dropwise mixed-cation solution is added drop-wise in lithium hydroxide solution.After ageing 20 h, cyclic washing is centrifugal for several times, then dry obtained presoma in drying box.To be dried complete after, grinding is evenly.Then stoichiometrically (excessive 5 wt.%) take lithium source lithium hydroxide, after mixing with presoma, and compressing tablet on powder compressing machine.In resistance furnace, sinter 6 h at 350 DEG C, at 1000 DEG C, sinter 18 h, obtained target product Li
1.13ni
0.22co
0.14mn
0.45al
0.05o
2, through the test as embodiment 1, specific discharge capacity 200 mAh/g can be obtained.
Embodiment 7:
After stoichiometrically taking nickel nitrate, cobalt nitrate, magnesium sulfate and manganese nitrate, add appropriate amount of deionized water and be mixed with the mixed solution that metal cation adds up to 0.1 M.Prepare the NaOH mixed solution of 0.2 M, and add 0.01M isopropyl alcohol.Control mixing speed, dropwise mixed-cation solution is added drop-wise in lithium hydroxide solution.After ageing 20 h, cyclic washing is centrifugal for several times, then dry obtained presoma in drying box.To be dried complete after, grinding is evenly.Then stoichiometrically (excessive 5 wt.%) take lithium source lithium hydroxide, after mixing with presoma, and compressing tablet on powder compressing machine.In resistance furnace, sinter 6 h at 350 DEG C, at 900 DEG C, sinter 12 h, at 1000 DEG C, sinter 8 h, obtained target product Li
1.13ni
0.22co
0.13mn
0.45mg
0.06o
2, through the test as embodiment 1, specific discharge capacity 189 mAh/g can be obtained.
Claims (1)
1. prepare the method for anode material of lithium battery for one kind, it is characterized in that: after stoichiometrically taking nickel acetate, cobalt acetate and manganese acetate, add appropriate amount of deionized water and be mixed with the mixed solution that metal cation adds up to 0.1 M, prepare the lithium hydroxide solution of 0.2 M, and add 0.01M ethanol/aqueous isopropanol, the ratio of ethanol and isopropyl alcohol is 1:1, controls mixing speed, is added drop-wise in lithium hydroxide solution by described metal cation mixed solution; After ageing 24 h, cyclic washing is centrifugal for several times, then dry obtained presoma in drying box, to be dried complete after, grinding is evenly; Then lithium source lithium hydroxide is taken by excessive 5 wt.%, after mixing with presoma, compressing tablet on powder compressing machine; 26 h are sintered at 900 DEG C, obtained target product Li in resistance furnace
1.09ni
0.29co
0.145mn
0.47o
2, stand-by after grinding;
Described target product Li in mass ratio
1.09ni
0.29co
0.145mn
0.47o
2: PVDF: after carbon black=85:8:7 takes each material, dry 12 h at 80 DEG C in vacuum drying chamber; The N-methyl measuring respective volume in the ratio of 1 g PVDF: 25 ml NMP adjoins pyrrolidone NMP, then with Kynoar PVDF mix and blend; After PVDF is fully swelling, by Li
1.09ni
0.29co
0.145mn
0.47o
2join in this solution with carbon black, continue to stir, until it mixes; Then after evenly smear is 16 mm aluminium flakes to diameter, dry in baking oven; Treat that positive plate is fully dry, compressing tablet, then dry 12 h at vacuum drying chamber 120 DEG C after removal NMP, put into glove box again and prepare assembling test after weighing;
Being assemblied in the glove box being full of argon gas of battery is carried out, and in the pre-assembly, is cleaned up by button cell shell with acetone, to remove the greasy dirt on surface, and dry 24 h; Assembly operation step is: place button cell cathode shell and lithium sheet successively, then drip electrolyte 1 M LiPF
6eC/DEC on lithium sheet, the example of EC/DEC is 1:1, places Celgard 2400 barrier film, then drips electrolyte on barrier film, finally places positive plate and anode cover; Seal on button cell sealing instrument, after placing 24 h hours, carry out the test of battery capacity performance; Carry out capacity test at 2-4.8V with 0.05C current density, specific discharge capacity reaches 200 mAh/g.
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KR101794097B1 (en) | 2013-07-03 | 2017-11-06 | 삼성에스디아이 주식회사 | Positive active material for rechargeable lithium battery, method of preparing the same, and positive electrode for rechargeable lithium battery and rechargeable lithium battery including the same |
CN103840216A (en) * | 2014-03-16 | 2014-06-04 | 辉县市玉杰科技有限公司 | Manufacturing method for lithium ion buckle type battery |
CN110776021B (en) * | 2019-11-27 | 2022-05-13 | 桑顿新能源科技有限公司 | Nickel cobalt lithium manganate positive electrode material and preparation method thereof, lithium ion battery positive electrode slurry, lithium ion battery positive electrode and lithium ion battery |
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CN101355159A (en) * | 2008-09-17 | 2009-01-28 | 金瑞新材料科技股份有限公司 | Method for preparing lithium ion battery anode material nickle cobalt lithium manganate |
CN101478044A (en) * | 2009-01-07 | 2009-07-08 | 厦门钨业股份有限公司 | Multi-element composite positive pole material for lithium secondary battery and preparation thereof |
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CN102244259A (en) * | 2011-06-17 | 2011-11-16 | 中国科学院化学研究所 | Composite lithium-rich anode material, its preparation method and its application |
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CN101355159A (en) * | 2008-09-17 | 2009-01-28 | 金瑞新材料科技股份有限公司 | Method for preparing lithium ion battery anode material nickle cobalt lithium manganate |
CN101478044A (en) * | 2009-01-07 | 2009-07-08 | 厦门钨业股份有限公司 | Multi-element composite positive pole material for lithium secondary battery and preparation thereof |
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