CN107275634A - A kind of method that high-tap density, the spherical lithium-rich manganese-based anode material of high power capacity are synthesized without complexing agent - Google Patents
A kind of method that high-tap density, the spherical lithium-rich manganese-based anode material of high power capacity are synthesized without complexing agent Download PDFInfo
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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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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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- 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 discloses a kind of method that high-tap density, the spherical lithium-rich manganese-based anode material of high power capacity are synthesized without complexing agent, comprise the following steps：1) nickel, cobalt, the mixed aqueous solution of the soluble-salt of manganese and precipitant solution are prepared；2) precipitant solution is measured, and adjusts the pH value of precipitant solution, and is heated；3) under stirring, the precipitating reagent cocurrent after nickel, cobalt, the mixed aqueous solution of the soluble-salt of manganese and heating is mixed, coprecipitation reaction；4) nickel cobalt manganese precipitation presoma is obtained after coprecipitated product washing, drying；5) complex oxide is obtained after the calcining of nickel cobalt manganese precipitation presoma；6) lithium carbonate is well mixed with complex oxide, by pre- calcination and sintering, produced.Using carbonate co-precipitation, under conditions of without complexing agent, the granular size and density of sintering process, effectively control presoma are improved, the spherical lithium-rich manganese-based anode material of high power capacity that tap density is big, energy density is big, high rate performance is good is prepared.
Description
Technical field
The invention belongs to the preparation of anode material for lithium-ion batteries, it is related specifically to a kind of without the high vibration density of complexing agent synthesis
Degree, the method for high power capacity lithium-rich manganese-based anode material.
Background technology
With the increasingly exhausted of fossil energy and the environmental problem faced at present, green and regenerative resource obtain more next
More research and concern.Battery quickly realizes the device that chemical energy and electric energy are mutually converted as a kind of, is rationally effectively sharp
With the important medium of the energy.Lithium ion battery is because its specific energy is high, operating voltage is high, operating temperature range is wide, storage life is long
Etc. advantage, it is widely used in fields such as mobile phone, notebook computer, video cameras.In addition, following hybrid power
(HEV) and the application in terms of pure electronic (EV) automobile, military affairs and space technology to the energy density of battery, power density and
Cycle life proposes higher requirement.Therefore, exploitation high-performance (high-energy-density, long-life, security), low cost lithium from
Sub- battery is the emphasis and focus of portable power source industry development, and Main way is exploitation suitable for the new of high performance lithium ion battery
Type electrode material and its technology of preparing.Recently, lithium-rich manganese-based anode material (Li1+x[NiαCoβMnγ]1-xO2, wherein alpha+beta+γ=
1) have the advantages that theoretical capacity is high, operating voltage is high, cost is low, have a safety feature, be expected to the high-energy as a new generation close
The anode material for lithium-ion batteries of degree.
The developing history of lithium ion battery is made a general survey of, can be clearly seen that the development of its electrode material exactly around raising
Energy density (mainly volume energy density) this demand expansion of battery.Improve the volume energy density of lithium ion battery
Mainly there is three approach：1) jolt ramming (compacting) density of positive electrode is improved；2) reversible specific capacity of positive electrode is improved；3) carry
The operating voltage of high positive electrode.Need triplicity in many cases.The jolt ramming (compacting) for improving positive electrode is close
Degree mainly has two methods, and first method is that material is prepared into micron-sized single crystal grain (10~20 μm), for example
The LiCoO of commercialization2And LiMn2O4.But, the material for being adapted to this method is few, and other contain various active transition metal group
The electrode material divided, such as nickel-cobalt-manganese ternary stratified material, it is difficult to be prepared into micron-sized large single crystal particle.In addition, nickel cobalt manganese
Ternary layered material is poor due to ionic conductivity, even if being prepared into micron-sized single crystal grain, its chemical property also can be big
Give a discount.For this problem, people develop the method that another improves positive electrode tap density, i.e., by once nanometer
The micron sphere material of particle assembling.This sphere material not only overcomes the problem of lithium ion spreads in micron single crystal grain,
Also greatly enhance the tap density of material.In addition, micron sphere material also has many other advantages, such as it is excellent
Different mobility, dispersiveness and processing characteristics.
At present, the micron sphere material for preparing high-tap density mainly uses coprecipitation, including hydroxide to be co-precipitated
Method, carbonate co-precipitation and oxalate coprecipitation method, wherein first two method are the most frequently used, and effect is also relatively good.Hydroxide
Coprecipitation is precipitating reagent typically using sodium hydroxide, and carbonate co-precipitation is then precipitating reagent, both sides using sodium carbonate
Method has respective advantage.In general, the primary particle of sphere material made from hydroxide precipitation method is larger, tap density compared with
High, specific surface area is small.But hydroxide precipitation, to air-sensitive, being oxidized easily causes nickel cobalt manganese isoreactivity in preparation process
Transition metal skewness in the material, so as to influence the chemical property of material.Therefore precipitation process needs inert gas
Protection, Coprecipitation is harsher.By contrast, carbonate in air-stable much, inoxidizability is strong, therefore is co-precipitated
Journey does not need inert gas shielding, and Coprecipitation compares mitigation.At present, prepared by coprecipitation needs in the spherical materials process of micron
Substantial amounts of complexing agent even surfactant is added, conventional complexing agent has sodium citrate, sodium tartrate, sulfosalicylic acid sodium salt
And ammoniacal liquor, wherein ammoniacal liquor is most widely used.In fact, these complexing agents are expensive, large-scale use not only improves the life of material
Cost is produced, can also increase the difficulty of final wash, the harm of the sewage of generation to environment is big, and cost of sewage disposal is high.For example it is special
Profit application CN103956479A describes a kind of preparation method of the spherical lithium-rich anode material of high power capacity.Used in preparation process
Ammoniacal liquor as complexing agent, and the material prepared tap density in 1.8g/cm-3Left and right.Patent application CN106410186A
A kind of preparation method of lithium-rich oxide anode material is described, the material is prepared using solid phase method, grain shape
Irregularly, and 40 circle circulation volumes in 240mAh g-1Left and right.
In summary, need to add greatly in the co-precipitation preparation method of spherical lithium-rich manganese-based anode material of the prior art
The complexing agent of amount, can not only improve the cost of positive electrode preparation, and the problem of also causing the pollution of environment still lacks effective
Solution.
The content of the invention
For above-mentioned problems of the prior art, high jolt ramming is synthesized without complexing agent it is an object of the invention to provide one kind
The method of the spherical lithium-rich manganese-based anode material of density, high power capacity.Using carbonate co-precipitation, under conditions of without complexing agent,
The granular size and density of sintering process, effectively control presoma are improved, prepares that tap density is big, energy density big, multiplying power
The spherical lithium-rich manganese-based anode material of high power capacity of excellent performance, the tap density of the positive electrode prepared can reach 2.4g/
cm-3。
In order to solve problem above, the technical scheme is that：
A kind of method that high-tap density, the spherical lithium-rich manganese-based anode material of high power capacity are synthesized without complexing agent, including it is as follows
Step：
1) nickel, cobalt, the mixed aqueous solution of the soluble-salt of manganese and the precipitant solution for setting concentration are prepared；
2) set amount 0.1-0.2mol L are measured-1Precipitating reagent be added in reactor as bottom liquid, it is and heavy with acid regulation
The pH value of shallow lake agent is 8.1-8.5, obtains concentration for 0.1-0.2mol L-1Cushioning liquid, cushioning liquid is heated；
3) under stirring, by nickel, cobalt, the mixed aqueous solution of the soluble-salt of manganese and 2-2.5mol L-1Precipitating reagent cocurrent is added
To step 2) in heat after cushioning liquid in, coprecipitation reaction, the mixing speed of coprecipitation reaction is 800-1200rpm, pH
It is worth for 8.1-8.5, charging rate is 200-500mlh-1, the reaction time is 8-12 hours；
4) after reaction terminates, coprecipitated product is washed with hot water, nickel cobalt manganese precipitation presoma is obtained after drying；
5) by the precipitation presoma calcining of obtained nickel cobalt manganese, complex oxide is obtained；
6) lithium carbonate is well mixed with complex oxide, by pre- calcination and sintering, obtains target product material.
Further, step 1) in, the precipitating reagent is one kind in sodium carbonate, potassium carbonate, sodium acid carbonate, saleratus
Or a variety of mixtures.
Further, step 1) in, nickel, cobalt, the soluble sulphate of manganese are its sulfate or nitrate.
Further, step 1) in, in nickel, cobalt, the mixed solution of manganese soluble sulphate, nickel, cobalt, the mol ratio of manganese are pressed
According to target compound (Li1+x(MnaNibCoc)1-xO2, wherein 0≤x≤0.2, a+b+c=1) and setting.
Further, step 2) in, described acid is the pH value that formic acid, acetic acid, propionic acid or butyric acid adjust cushioning liquid,
Organic acid is easy to remove during subsequent calcination.
Further, step 2) in, cushioning liquid is as bottom liquid, and the temperature after heating is 50-70 DEG C.
Further, step 4) in, it is 40-60 to be washed coprecipitated product to the temperature close to neutrality, hot water with hot water
℃。
Further, step 4) in, the temperature that coprecipitated product is dried is 105-115 DEG C, and the dry time is 10-13h.
Further, step 5) in, the temperature of nickel cobalt manganese precipitation presoma calcining is 450-500 DEG C, and the time of calcining is
8-14h。
Further, step 6) in, the temperature being calcined in advance is 480-520 DEG C, and the time being calcined in advance is 1.5-2.5h.
Further, step 6) in, the temperature of sintering is 880-920 DEG C, and the programming rate between pre- calcination and sintering is 2
℃ min-1.Target product material Li is obtained after cooling1+x(MnaNibCoc)1-xO2, wherein 0≤x≤0.2, a+b+c=1.
The spherical lithium-rich manganese-based anode material Li that above-mentioned preparation method is prepared1+x(MnaNibCoc)1-xO2, wherein 0≤x
≤ 0.2, a+b+c=1.
Beneficial effects of the present invention are：
Using carbonate co-precipitation, under conditions of without complexing agent, of sintering process, effectively control presoma is improved
Grain size and density, prepare the spherical lithium-rich manganese-based anode material of high power capacity that tap density is big, energy density is big, high rate performance is good
Expect Li1+x(MnaNibCoc)1-xO2, wherein 0≤x≤0.2, a+b+c=1, the tap density of positive electrode can reach 2.4g/cm-3。
Brief description of the drawings
The Figure of description for constituting the part of the application is used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its illustrate be used for explain the application, do not constitute the improper restriction to the application.
Fig. 1 is the spherical lithium-rich anode material presoma carbonate SEM that embodiment 1 is prepared using the sulfate of nickel, cobalt, manganese
Figure.
Fig. 2 is high-tap density, the spherical rich lithium manganese of high power capacity that presoma prepared by embodiment 1 is prepared using calcine technology
Base anode material Li1.2Mn0.54Ni0.14Co0.12O2SEM figure.
Fig. 3 is lithium-rich manganese-based anode material Li prepared by embodiment 11.2Mn0.54Ni0.14Co0.12O2XRD.
Fig. 4 is lithium-rich manganese-based anode material Li prepared by embodiment 11.2Mn0.54Ni0.14Co0.12O2Cycle performance curve.
Embodiment
It is noted that described further below is all exemplary, it is intended to provide further instruction to the application.Unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
Embodiment 1
Using intermittent reaction pattern, by manganese sulfate, nickel sulfate and cobaltous sulfate proportionally 37:7:6 proportions are into total
Concentration is 2M mixed solution, in the homemade reactors of 2L, adds 200mL 0.1mol L-1Sodium carbonate liquor, add vinegar
Acid regulation 8.3 or so, is heated to 60 DEG C.Under stirring, by nickel, cobalt, manganese 500 milliliters of sulfate and 2.1mol L-1Sodium carbonate
476 milliliters of cocurrents of precipitating reagent, which are added in reactor, reacts, and the mixing speed for controlling precipitation process is 100-1000 rpm, pH value
It is 250mL h for 8.2-8.5, charging rate-1, total reaction time is 12 hours.Reaction terminates, and is washed precipitated product with hot water
To close to neutrality, then 110 DEG C of drying 12 hours obtain nickel cobalt manganese and precipitate presoma.Resulting spherical precursor material exists
Calcining is converted into complex oxide in 8 hours at 500 DEG C, further according to lithium ion in target product and the ratio (Li/ of transition metal
M=(1+x)/(1-x), lithium carbonate is well mixed with complex oxide.First in 500 DEG C of precalcinings 2 hours in Muffle furnace,
Then calcined 1 hour at 900 DEG C, programming rate is 2 DEG C of min-1, target product material is obtained after cooling
Li1.2Mn0.54Ni0.14Co0.12O2, the tap density of material is 2.4g/cm-3。
Fig. 1 is the spherical lithium-rich anode material presoma carbonate SEM that embodiment 1 is prepared using the sulfate of nickel, cobalt, manganese
Figure, it can be seen that the response parameter by optimizing and controlling coprecipitation process, can obtain preferable spherical morphology
Carbonate precursor material, particle diameter distribution is narrower, and average grain diameter is 14 μm or so.Fig. 2 is that presoma prepared by embodiment 1 is used
High-tap density, the spherical lithium-rich manganese-based anode material Li of high power capacity of calcine technology preparation1.2Mn0.54Ni0.14Co0.12O2SEM
Figure.Fig. 3 is lithium-rich manganese-based anode material Li prepared by embodiment 11.2Mn0.54Ni0.14Co0.12O2XRD.From Fig. 2 and Fig. 3
As can be seen that being sintered under the program, the spherical of material is kept well, and with more preferable crystallinity and stratiform
Structural intergrity.
Fig. 4 is lithium-rich manganese-based anode material Li prepared by embodiment 11.2Mn0.54Ni0.14Co0.12O2Cycle performance curve.
Embodiment 2
Using successive reaction pattern, by manganese sulfate, nickel sulfate and cobaltous sulfate proportionally 37:7:6 proportions are into total
Concentration is 2M mixed solution, in the homemade reactors of 10L, adds 1000mL 0.1mol L-1Sodium carbonate liquor, add
Acetic acid regulation 8.3 or so, is heated to 60 DEG C.Under stirring, by nickel, cobalt, manganese 2.5 liters of sulfate and 2.1mol L-1Sodium carbonate
Precipitating reagent (2.38 liters) cocurrent, which is added in reactor, reacts, and the mixing speed for controlling precipitation process is 100-1000rpm, pH
Value is that 8.2~8.5, charging rate is 250mL h-1, the reaction time is that after 12 hours, discharging to reactor midsole liquid is 1000 millis
Rise, proceed reaction.Reaction terminates, and is washed the precipitated product of many secondary responses to close to neutrality with hot water, then done for 110 DEG C
Dry 12 hours, obtain nickel cobalt manganese precipitation presoma.Resulting spherical precursor material is calcined 8 hours at 500 DEG C and is converted into
Complex oxide, further according to ratio (Li/M=(1+x)/(1-x), by carbonic acid of lithium ion in target product and transition metal
Lithium is well mixed with complex oxide.First 500 DEG C of precalcinings 2 hours, are then calcined 1 hour at 900 DEG C in Muffle furnace,
Programming rate is 2 DEG C of min-1, target product material Li is obtained after cooling1.2Mn0.54Ni0.14Co0.12O2, the tap density of material is
2.4g/cm-3。
The preferred embodiment of the application is the foregoing is only, the application is not limited to, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. a kind of method that high-tap density, the spherical lithium-rich manganese-based anode material of high power capacity are synthesized without complexing agent, it is characterised in that：
Comprise the following steps：
1) nickel, cobalt, the mixed aqueous solution of the soluble-salt of manganese and the precipitant solution for setting concentration are prepared；
2) set amount 0.1-0.2mol L are measured-1Precipitating reagent be added in reactor as bottom liquid, and with acid adjust precipitating reagent
PH value be 8.1-8.5, obtain concentration for 0.1-0.2mol L-1Cushioning liquid, cushioning liquid is heated；
3) under stirring, by nickel, cobalt, the mixed aqueous solution of the soluble-salt of manganese and 2-2.5mol L-1Precipitating reagent cocurrent is added to step
In cushioning liquid after rapid 2) middle heating, coprecipitation reaction, the mixing speed of coprecipitation reaction is 800-1200rpm, and pH value is
8.1-8.5, charging rate is 200-500mlh-1, the reaction time is 8-12 hours；
4) after reaction terminates, coprecipitated product is washed with hot water, nickel cobalt manganese precipitation presoma is obtained after drying；
5) by the precipitation presoma calcining of obtained nickel cobalt manganese, complex oxide is obtained；
6) lithium carbonate is well mixed with complex oxide, by pre- calcination and sintering, obtains target product material.
2. according to the method described in claim 1, it is characterised in that：Step 1) in, the precipitating reagent be sodium carbonate, potassium carbonate,
One or more mixtures in sodium acid carbonate, saleratus.
3. according to the method described in claim 1, it is characterised in that：Step 1) in, nickel, cobalt, the soluble sulphate of manganese are it
Sulfate or nitrate.
4. according to the method described in claim 1, it is characterised in that：Step 1) in, nickel, cobalt, the mixing of manganese soluble sulphate
In solution, nickel, cobalt, the mol ratio of manganese are according to target compound (Li1+x(MnaNibCoc)1-xO2, wherein 0≤x≤0.2, a+b+c
=1) set.
5. according to the method described in claim 1, it is characterised in that：Step 2) in, use formic acid, acetic acid, propionic acid or butyric acid
Adjust the pH value of precipitating reagent.
6. according to the method described in claim 1, it is characterised in that：Step 2) in, the temperature after heating is 50-70 DEG C.
7. according to the method described in claim 1, it is characterised in that：Step 4) in, the temperature that coprecipitated product is dried is 105-
115 DEG C, the dry time is 10-13h.
8. according to the method described in claim 1, it is characterised in that：Step 5) in, the temperature of nickel cobalt manganese precipitation presoma calcining
For 450-500 DEG C, the time of calcining is 8-14h.
9. according to the method described in claim 1, it is characterised in that：Step 6) in, the temperature being calcined in advance is 480-520 DEG C, in advance
The time of calcination is 1.5-2.5h；The temperature of sintering is 880-920 DEG C, and the programming rate between pre- calcination and sintering is 2 DEG C
min-1。
10. the spherical lithium-rich manganese-based anode material Li that any methods describeds of claim 1-9 are prepared1+x(MnaNibCoc)1- xO2, wherein 0≤x≤0.2, a+b+c=1.
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| CN111498908A (en) * | 2020-04-27 | 2020-08-07 | 中信大锰矿业有限责任公司 | Preparation method of quasi-spherical manganese-rich ternary precursor |
| CN111987305A (en) * | 2020-08-28 | 2020-11-24 | 四川虹微技术有限公司 | Method for preparing high-capacity lithium-rich manganese-based positive electrode material through ammoniation-free coprecipitation |
| CN112786876A (en) * | 2021-03-02 | 2021-05-11 | 昆明理工大学 | Preparation method of lithium-rich lithium battery cathode material with single crystal structure |
| CN113036095A (en) * | 2020-03-27 | 2021-06-25 | 湖南杉杉能源科技股份有限公司 | Preparation method of single-crystal-morphology lithium ion battery positive electrode material |
| CN114665086A (en) * | 2022-02-18 | 2022-06-24 | 中国科学院青海盐湖研究所 | Lithium-rich manganese-based positive electrode material and preparation method thereof |
| CN114906881A (en) * | 2022-04-29 | 2022-08-16 | 浙江格派钴业新材料有限公司 | Preparation method of cation-substituted modified spherical-like sodium nickel manganese oxide positive electrode material |
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| 张彦涛: "锂离子电池正极材料Li1.2(Ni0.133Co0.133Mn0.533)O2的制备及性能研究", 《工程科技II辑》 * |
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| CN111987305A (en) * | 2020-08-28 | 2020-11-24 | 四川虹微技术有限公司 | Method for preparing high-capacity lithium-rich manganese-based positive electrode material through ammoniation-free coprecipitation |
| CN112786876A (en) * | 2021-03-02 | 2021-05-11 | 昆明理工大学 | Preparation method of lithium-rich lithium battery cathode material with single crystal structure |
| CN114665086A (en) * | 2022-02-18 | 2022-06-24 | 中国科学院青海盐湖研究所 | Lithium-rich manganese-based positive electrode material and preparation method thereof |
| CN114906881A (en) * | 2022-04-29 | 2022-08-16 | 浙江格派钴业新材料有限公司 | Preparation method of cation-substituted modified spherical-like sodium nickel manganese oxide positive electrode material |
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