CN102163713A - Method for preparing high-voltage spinel anode material of lithium-ion secondary battery - Google Patents

Method for preparing high-voltage spinel anode material of lithium-ion secondary battery Download PDF

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CN102163713A
CN102163713A CN2011100647446A CN201110064744A CN102163713A CN 102163713 A CN102163713 A CN 102163713A CN 2011100647446 A CN2011100647446 A CN 2011100647446A CN 201110064744 A CN201110064744 A CN 201110064744A CN 102163713 A CN102163713 A CN 102163713A
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manganese
lithium
nickel
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施志聪
陈国华
张玲玉
邓胜男
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Guangzhou HKUST Fok Ying Tung Research Institute
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Abstract

The invention relates to a method for preparing a high-voltage spinel anode material LiMxNi0.5-xMn1.5O4 of a lithium-ion secondary battery (M=Mg, Fe, Zn, Cu, Co, Ce and La, and x is more than or equal to 0 and less than or equal to 0.2). The method comprises the following steps of: reacting nickel salt, manganese salt and doped metal salt with oxalate, and co-precipitating to obtain a metal oxalate precursor; fully mixing the precursor and lithium salt and preburning at the temperature of 550 DEG C for 5 to 10 hours; and calcining at the temperature of between 800 and 950 DEG C for 12 to 24 hours, naturally cooling to room temperature, and grinding to obtain the high-voltage spinel anode material LiMxNi0.5-xMn1.5O4. The anode material LiMxNi0.5-xMn1.5O4 prepared by the method is high in voltage platform, stable in performance, low in cost, environment-friendly and suitable for expanded reproduction, and has no special requirement on experimental environment.

Description

A kind of preparation method of lithium rechargeable battery high voltage spinelle positive electrode
Technical field
The present invention relates to a kind of lithium rechargeable battery high voltage spinelle positive electrode LiM xNi 0.5-xMn 1.5O 4(M=Mg, Fe, Zn, Cu, Co, Ce, La; 0≤x≤0.2) preparation method belongs to the high-performance lithium ion secondary battery technology.
Background technology
Lithium rechargeable battery occupies the consumption market rapidly with its superior performance, and is considered to the major impetus energy of electric automobile of future generation and hybrid-electric car.The many positive electrodes of research mainly contain the LiCoO of layer structure at present 2, LiNiO 2, LiMn xCo yNi 1-x-yO 2, the LiMn of spinel structure 2O 4, the LiFePO of olivine-type structure 4Deng.LiCoO 2Though battery energy density height, good temp characteristic, the safety problem of cost height, product is troubling; LiFePO 4The Product Safety of battery is far above LiCoO 2Battery, but the conduction problem is still waited to improve; Though lithium-nickel-cobalt-oxygen system battery capacity is improved, and can't solve safety issue fully; Though the spinel lithium manganate battery is safe, the short obstacle that becomes its development of hot properties and life-span.In recent years, improve the cell positive material technology with improving safety, to increase the battery charge capacity and reduce cost be the major axes orientation of lithium rechargeable battery development.Be accompanied by very big demand and the high voltage electrolyte and the electrolytical research success of electric automobile, high voltage spinel LiM xNi 0.5-xMn 1.5O 4(M=Mg, Fe, Zn, Cu, Co, Ce, La; 0≤x≤0.2) received great concern.Recent studies show that at above-mentioned various high voltage spinels the high voltage platform is arranged not only, and have fail safe preferably and cycle performance.
The method of synthetic above-mentioned spinel structure material mainly contains high-temperature solid phase reaction method, sol-gel process, gel combustion method and coprecipitation etc.High-temperature solid phase reaction method is with directly ball milling mixing such as lithium source, nickel source, manganese source, calcining at high temperature.This method is simple to operation, but it is inhomogeneous to occur batch mixing in the preparation process easily, causes product structure, phenomenon that particle size differences is big, and the chemical property of material is also wayward, batch and batch between difference big.Though the synthetic product of sol-gel process can evenly mix, the purity height, crystal property is good, and initial capacity is higher, and cycle performance is also better, and synthesis material generally adopts organic reagent, and cost is higher, so be difficult to practical application.Method the most general, that have application prospect most is co-precipitation-solid-phase synthesis at present.Adopt coprecipitation to prepare persursor material, again presoma is mixed with the lithium source,, finally obtain spinelle nickel manganese lithium material through high-temperature heat treatment.Precipitation reagent mainly contains NaOH and sodium carbonate; because the hydroxide of manganese is very unstable; as easy as rolling off a log oxidation; need inert gas shielding; the formation of its nucleus and developmental process are difficult to control; so NaOH prepares the method technology controlling and process complexity of presoma as precipitation reagent, is unfavorable for large batch of suitability for industrialized production.Adopt sodium carbonate can directly calcine under air atmosphere as the synthetic presoma of precipitation reagent, simple to operation, cost is low, and the precipitation reagent of common comparative maturity is exactly a sodium carbonate on the document at present.Consider the problem of difficult washing of sodium ion and the control of pH value, we adopt ammonium oxalate to synthesize LiM as precipitation reagent first xNi 0.5-xMn 1.5O 4(M=Mg, Fe, Zn, Cu, Co, Ce, La; 0≤x≤0.2).The method cost is lower and easy and simple to handle equally, and experimental situation is not had specific (special) requirements, and environmental friendliness, is applicable to enlarged reproduction.
Summary of the invention
The object of the present invention is to provide a kind of employing ammonium oxalate as the synthetic high voltage spinelle positive electrode LiM of precipitation reagent xNi 0.5-xMn 1.5O 4(M=Mg, Fe, Zn, Cu, Co, Ce, La; 0≤x≤0.2) preparation method.By conditions such as control temperature, mixings time, generate the metal oxalate presoma precipitation of composition and even particle size distribution, high-temperature calcination in air atmosphere obtains high voltage spinelle positive electrode LiM with this presoma and lithium source xNi 0.5-xMn 1.5O 4
The method that realizes above-mentioned purpose is co-precipitation-high temperature solid-state method, the LiM of this method preparation xNi 0.5-xMn 1.5O 4The highest specific discharge capacity can reach 130 mAh g -1More than, circulation 30 circle back capability retentions are up to more than 90%.
Preparation technology's key step of the present invention is as follows:
Step 1, nickel salt, manganese salt and metal M salt are mixed in deionized water, be mixed with [Mn 2++ Ni 2++ M N+] the metal ion total concentration is the mixing salt solution 1 of 0.5mol/L, wherein manganese salt: nickel salt: the mol ratio of M salt is 1.5:0.5-x:x (0≤x≤0.2);
The isocyatic ammonium oxalate solution of step 2, preparation and mixing salt solution equal-volume 2 is as precipitation reagent;
Step 3, with solution 1 and solution 2 hybrid reactions, 55 ℃～60 ℃ of control reaction temperature and reaction time 6h～12h obtain the presoma precipitation;
Step 4, the product of step 3 gained is obtained nickel manganese metal M oxalates presoma through suction filtration, drying behind ultrasonic washing and the deionized water wash successively;
Step 5, the presoma of lithium salts and step 4 gained is ground evenly, place 550 ℃ of pre-burning 5h ~ 10h of Muffle furnace, be warmed up to 800 ℃～950 ℃ sintering 12 ~ 24h again, wherein take by weighing excessive 3% ~ 6% lithium salts according to the mol ratio of lithium salts and presoma;
Step 6, the cooling of the calcined product of step 5 gained ground promptly obtain high voltage spinelle positive electrode LiM xNi 0.5-xMn 1.5O 4(M=Mg, Fe, Zn, Cu, Co, Ce, La; 0≤x≤0.2).
The manganese salt that the present invention adopts is a kind of or its salt-mixture in manganese sulfate, manganese acetate, manganese carbonate, manganese nitrate, manganese chloride, the manganese oxalate.
The nickel salt that the present invention adopts is a kind of or its salt-mixture in nickelous sulfate, nickel acetate, nickelous carbonate, nickel nitrate, nickel chloride, the nickel oxalate.
The metal M salt that the present invention adopts is a kind of or its salt-mixture in the sulfate, acetate, carbonate, nitrate, villaumite, oxalates of M.
The precipitation reagent that the present invention adopts is an ammonium oxalate.
The solvent that the present invention adopts is a deionized water.
The lithium salts that the present invention adopts is a kind of or its salt-mixture in lithium carbonate, lithium sulfate, lithium nitrate, lithium hydroxide, the lithium acetate etc.
Advantage of the present invention and positive effect are:
Whole technology is very simple, and is easy to operate, and solvent is deionized water, and is environmentally friendly;
Synthetic material purity height, good dispersion, required time is short;
Cost is low, and experimental situation is not had specific (special) requirements, and synthetic material property is stable, is fit to enlarged reproduction.
Description of drawings
Fig. 1 is the SEM figure of nickel manganese oxalates presoma co-precipitation, and granular precursor is even as seen from the figure, and the primary particle particle diameter is about 6 μ m.
Fig. 2 generates LiNi for nickel manganese oxalates presoma after through 800 ℃, 900 ℃ high-temperature calcinations 0.5Mn 1.5O 4SEM figure, smaller through the material primary particle after 800 ℃ of calcinings as seen from the figure, and the trend that is agglomerated into second particle is arranged; Through the primary particle particle diameter after 900 ℃ of calcinings is that agglomeration is very slight about 4 μ m, and particle size distribution is more even.
Fig. 3 generates LiNi for nickel manganese oxalates presoma after through 800 ℃, 900 ℃ calcinings 0.5Mn 1.5O 4Specific discharge capacity curve chart (0.1C), the maximum specific discharge capacity of the material after two each and every one the temperature calcinings is respectively as seen from the figure: 136 mAh g -1, 124 mAh g -1Higher through the material after 800 ℃ of calcinings, but along with the increase that discharges and recharges number of times at preceding 25 circle capacity, present than advantages of higher stability through the material of 900 ℃ of calcinings, 30 circle circulation back capability retentions are 92.8%.
Fig. 4 generates LiNi for nickel manganese oxalates presoma after through 800 ℃, 900 ℃ calcinings 0.5Mn 1.5O 4High rate performance figure, be better than material high rate performance through the high rate performance of the material after 800 ℃ of calcinings as seen from the figure through 900 ℃ of calcinings.
Fig. 5 generates LiNi for nickel manganese oxalates presoma after through 900 ℃ of calcinings 0.5Mn 1.5O 4Charging and discharging curve figure.
Fig. 6 generates LiMg for nickel manganese magnesium oxalates presoma after through 900 ℃ of calcinings 0.1Ni 0.4Mn 1.5O 4The specific discharge capacity curve chart.
Fig. 7 generates LiMg for nickel manganese magnesium oxalates presoma after through 900 ℃ of calcinings 0.1Ni 0.4Mn 1.5O 4High rate performance figure.
Fig. 8 generates LiCe for nickel manganese cerium oxalates presoma after through 900 ℃ of calcinings 0.05Ni 0.45Mn 1.5O 4High rate performance figure.
Fig. 9 be nickel manganese oxalates presoma through 900 ℃ of calcinings after the XRD figure of material, this material is the Fd3m spinel structure as seen from the figure, also has minor N iO impurity in the material.
Embodiment
Below introduce content of the present invention in detail for specific embodiment, it is for the ease of understanding the present invention that embodiment is provided, and never is the invention of restriction this patent.
LiM provided by the present invention xNi 0.5-xMn 1.5O 4(M=Mg, Fe, Zn, Cu, Co, Ce, La; 0≤x≤0.2) in lithium ion battery, uses as positive electrode in the preparation.
Embodiment 1
X=0 in the present embodiment is 0.5mol/L(200ml with manganese sulfate, nickelous sulfate preparation total concentration) mixing salt solution 1, manganese salt wherein: the mol ratio of nickel salt is 1.5:0.5, prepares 0.5mol/L(200ml simultaneously) ammonium oxalate solution 2.With solution 1 and solution 2 hybrid reactions, 55 ℃ of reactions of control reaction temperature 10h obtains coprecipitate, and the coprecipitate with gained obtains nickel manganese oxalates presoma through suction filtration, drying behind ultrasonic washing, the deionized water wash successively then.Nickel manganese oxalates presoma with lithium salts and above-mentioned gained grinds evenly again, place 550 ℃ of pre-burning 5h of Muffle furnace, be warmed up to 800 ℃ of sintering 12h again, naturally cool to room temperature (wherein take by weighing excessive 6% lithium salts), will grind through the cooled product of calcining at last and promptly obtain high voltage spinelle positive electrode LiMn according to the mol ratio of lithium salts and presoma 1.5Ni 0.5O 4
Embodiment 2
X=0 in the present embodiment is 0.5mol/L(200ml with manganese sulfate, nickelous sulfate preparation total concentration) mixing salt solution 1, manganese salt wherein: the mol ratio of nickel salt is 1.5:0.5, prepares 0.5mol/L(200ml simultaneously) ammonium oxalate solution 2.With solution 1 and solution 2 hybrid reactions, 55 ℃ of reactions of control reaction temperature 10h obtains coprecipitate, and the coprecipitate with gained obtains nickel manganese oxalates presoma through suction filtration, drying behind ultrasonic washing, the deionized water wash successively then.Nickel manganese oxalates presoma with lithium salts and above-mentioned gained grinds evenly again, place 550 ℃ of pre-burning 5h of Muffle furnace, be warmed up to 900 ℃ of sintering 12h again, naturally cool to room temperature (wherein take by weighing excessive 6% lithium salts), will grind through the cooled product of calcining at last and promptly obtain high voltage spinelle positive electrode LiMn according to the mol ratio of lithium salts and presoma 1.5Ni 0.5O 4
Embodiment 3
X=0.1, M=Mg in the present embodiment, with manganese sulfate, nickelous sulfate, magnesium acetate preparation total concentration is 0.5mol/L(200ml) mixing salt solution 1, manganese salt wherein: nickel salt: the mol ratio of magnesium salts is 1.5:0.4:0.1, prepares 0.5mol/L(200ml simultaneously) ammonium oxalate solution 2.With solution 1 and solution 2 hybrid reactions, 55 ℃ of reactions of control reaction temperature 10h obtains coprecipitate, and the coprecipitate with gained obtains nickel manganese magnesium oxalates presoma through suction filtration, drying behind ultrasonic washing, the deionized water wash successively then.Nickel manganese magnesium oxalates presoma with lithium salts and above-mentioned gained grinds evenly again, place 550 ℃ of pre-burning 5h of Muffle furnace, be warmed up to 900 ℃ of sintering 12h again, naturally cool to room temperature (wherein take by weighing excessive 6% lithium salts), will grind through the cooled product of calcining at last and promptly obtain high voltage spinelle positive electrode LiMn according to the mol ratio of lithium salts and presoma 1.5Ni 0.4Mg 0.1O 4
Embodiment 4
X=0.05, M=Ce in the present embodiment, with manganese sulfate, nickelous sulfate, cerous nitrate preparation total concentration is 0.5mol/L(200ml) mixing salt solution 1, manganese salt wherein: nickel salt: the mol ratio of cerium salt is 1.5:0.45:0.05, prepares 0.5mol/L(200ml simultaneously) ammonium oxalate solution 2.With solution 1 and solution 2 hybrid reactions, 55 ℃ of reactions of control reaction temperature 10h obtains coprecipitate, and the coprecipitate with gained obtains nickel manganese magnesium oxalates presoma through suction filtration, drying behind ultrasonic washing, the deionized water wash successively then.Nickel manganese magnesium oxalates presoma with lithium salts and above-mentioned gained grinds evenly again, place 550 ℃ of pre-burning 5h of Muffle furnace, be warmed up to 900 ℃ of sintering 12h again, naturally cool to room temperature (wherein take by weighing excessive 6% lithium salts), will grind through the cooled product of calcining at last and promptly obtain high voltage spinelle positive electrode LiCe according to the mol ratio of lithium salts and presoma 0.05Ni 0.45Mn 1.5O 4
Above-mentioned concrete execution mode is an optimum execution mode of the present invention; especially ammonium oxalate is as precipitation reagent and calcining heat; but can not limit claim of the present invention, other is any not to deviate from technical scheme of the present invention and is included in protection scope of the present invention.

Claims (8)

1. lithium rechargeable battery high voltage spinelle positive electrode LiM xNi 0.5-xMn 1.5O 4(M=Mg, Fe, Zn, Cu, Co, Ce, La; 0≤x≤0.2) preparation method is characterized in that adopting first ammonium oxalate to generate a kind of particle as precipitation reagent and forms that speed is fast, the nickel manganese metal oxalate presoma of even particle size distribution.
2. high voltage spinelle positive electrode LiM according to claim 1 xNi 0.5-xMn 1.5O 4(M=Mg, Fe, Zn, Cu, Co, Ce, La; 0≤x≤0.2) preparation method, its feature mainly may further comprise the steps:
Step 1, step 1, nickel salt, manganese salt and metal M salt are mixed in deionized water, be mixed with [Mn 2++ Ni 2++ M N+] the metal ion total concentration is the mixing salt solution 1 of 0.5mol/L, wherein manganese salt: nickel salt: the mol ratio of M salt is 1.5:0.5-x:x (0≤x≤0.2);
The isocyatic ammonium oxalate solution of step 2, preparation and mixing salt solution equal-volume 2 is as precipitation reagent;
Step 3, with solution 1 and solution 2 hybrid reactions, 55 ℃～60 ℃ of control reaction temperature and reaction time 6h～12h obtain the presoma precipitation;
Step 4, the product of step 3 gained is obtained nickel manganese metal M oxalates presoma through suction filtration, drying behind ultrasonic washing and the deionized water wash successively;
Step 5, the presoma of lithium salts and step 4 gained is ground evenly, place 550 ℃ of pre-burning 5h ~ 10h of Muffle furnace, be warmed up to 800 ℃～950 ℃ sintering 12 ~ 24h again, wherein take by weighing excessive 3% ~ 6% lithium salts according to the mol ratio of lithium salts and presoma;
Step 6, the cooling of the calcined product of step 5 gained ground promptly obtain high voltage spinelle positive electrode LiM xNi 0.5-xMn 1.5O 4(M=Mg, Fe, Zn, Cu, Co, Ce, La; 0≤x≤0.2).
3. preparation method as claimed in claim 2 is characterized in that manganese salt is a kind of or its salt-mixture in manganese sulfate, manganese acetate, manganese carbonate, manganese nitrate, manganese chloride, the manganese oxalate, and what this experiment was adopted is manganese sulfate.
4. preparation method as claimed in claim 2 is characterized in that nickel salt is a kind of or its salt-mixture in nickelous sulfate, nickel acetate, nickelous carbonate, nickel nitrate, nickel chloride, the nickel oxalate, and what this experiment was adopted is nickelous sulfate.
5. preparation method as claimed in claim 2 is characterized in that metal M salt is a kind of or its salt-mixture in the sulfate, acetate, carbonate, nitrate, villaumite, oxalates of M, and what this experiment was adopted is magnesium acetate.
6. preparation method as claimed in claim 2 is characterized in that precipitation reagent is sodium carbonate, NaOH, ammonium carbonate, ammonium oxalate etc., the ammonium oxalate that this experiment is adopted.
7. preparation method as claimed in claim 2 is characterized in that the solvent that this experiment is adopted is a deionized water.
8. preparation method as claimed in claim 2 is characterized in that lithium salts is lithium carbonate, lithium sulfate, lithium nitrate, lithium hydroxide, lithium acetate etc., and what this experiment was adopted is lithium carbonate.
CN2011100647446A 2011-03-17 2011-03-17 Method for preparing high-voltage spinel anode material of lithium-ion secondary battery Pending CN102163713A (en)

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CN102569776A (en) * 2011-12-30 2012-07-11 合肥国轩高科动力能源有限公司 Preparation method of spinel type lithium manganese oxide for spherical high-voltage anode material
CN102730761A (en) * 2012-06-18 2012-10-17 中国第一汽车股份有限公司 Oxalate coprecipitation preparation method for high-capacity lithium-rich cathode material
CN102738453A (en) * 2012-07-11 2012-10-17 中国第一汽车股份有限公司 High-tap-density lithium-enriched material prepared by using hydroxyl coprecipitation-fused salt method
CN102875130A (en) * 2012-10-15 2013-01-16 福建师范大学 Method for preparing doped lithium-enriched solid solution cathode material by using carbon-added compound
CN102903897A (en) * 2012-07-20 2013-01-30 合肥国轩高科动力能源有限公司 Method for preparing nickel lithium manganate having spinel structure by static mixer type reactor
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Application publication date: 20110824