CN103515590A - Preparation method of ternary anode material of lithium ion battery - Google Patents
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- 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
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- 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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Abstract
A preparation method of a ternary anode material of a lithium ion battery comprises the steps of: 1) uniformly mixing nickel salt, cobalt salt, manganese salt, and a lithium compound at a stoichiometric ratio of (2-6):(2-3):(2-4):1, 2) grinding for 2-8h by taking alcohol as a grinding medium, 3) drying a mixture ground in Step 2) at 100-120 DEG C, obtaining reaction powder, 4) applying plasma electric arc on the reaction powder to fuse the reaction powder, and 5) injecting the fusion reaction powder into a cooling device with oxidizing gas, and forming a spherical fine particle through oxidation and cooling. With the adoption of the preparation method of the ternary material, the ternary anode material can be synthesized quickly and conveniently, is regular in morphology, is highly spherical, and has stable electrochemical performances, high purity and uniform components. According to the method, the ternary anode material with the uniform components and stable performances can be quickly synthesized through plasma high-temperature fusion of ingredients.
Description
Technical field
The present invention relates to electrode material field, be specifically related to a kind of manufacture method of ternary layered structure electrode material.
Background technology
Lithium ion battery is new generation of green high-energy battery, the many merits such as have that voltage is high, energy density is large, good cycle, self discharge are little, memory-less effect, operating temperature range are wide, be widely used in phone, notebook computer, electric tool etc., in electric automobile, also have a good application prospect, be it is believed that it is significant high energy technical products of 21 century.Recently, the Li[Ni-Co-Mn of ternary layered structure] O
2anode material for lithium-ion batteries is due to its high discharge capacity, good security performance, and the focus of advantage the becomes current research such as toxicity is little.It combines LiCoO
2good cycle performance, LiNiO
2high discharge capacity, and LiMnO
2excellent security performance, becomes high-energy-density Li-ion battery for HEV positive electrode, but its cycle performance and high-rate charge-discharge capability need further to be improved.Along with such material is in the innovation aspect preparation method, as going deep into of the aspect researchs such as finishing, morphology Control and raising tap density, and the improving constantly and improve of performance, tertiary cathode material develops into the main positive electrode of current lithium electricity application gradually, becomes the LiCoO that continues
2, very promising lithium ion battery novel anode material after LiFePO4.
Existing Li[Ni-Co-Mn] O
2the preparation method of anode material for lithium-ion batteries has solid phase method, coprecipitation and microwave method etc.Solid phase method synthesis of ternary positive electrode, is exactly mainly Ni, Co, the oxide of tri-kinds of transition metal of Mn and mixing with Li salt, carries out calcination at a certain temperature, can synthesize final product Li[Ni-Co-Mn] O
2.For example Chinese patent CN1956244, CN102169990A, CN102779992A, CN101139108, but the chemical property of the ternary material that this method is made has obvious deficiency, particularly specific capacity and cycle performance all obviously poor.Coprecipitation is the main method of synthesis of ternary material.The presoma chemical property that this method makes is good, and dry rear powder granule is even, and after calcining, performance is good.Shortcoming is that reaction time is long, and equipment is complicated, and reaction factor is wayward, and suitability for industrialized production uncertain factor is more.For example Chinese patent CN101083321, CN101863519A.What microwave method made is mainly a kind of microwave heating method, by Ni, Co, the oxide of tri-kinds of transition metal of Mn and and Li salt carry out carrying out microwave heating with certain heating rate after mixing, obtain end product.For example Chinese patent CN101967055A, CN102157725A, this method is simple, easy to control, simple to operate, but the end product structure obtaining is inhomogeneous, and chemical property is general.The industrialized batch production of the ternary material that these problems all restrict, and corresponding economic benefit.
The ternary material of applying now mainly contains several, by the ratio changing between transition metal, can be divided into LiNi
0.3co
0.3mn
0.3o
2, LiNi
0.5co
0.2mn
0.3o
2, LiNi
0.4co
0.4mn
0.2o
2, LiNi
0.6co
0.2mn
0.2o
2, LiNi
0.8co
0.1mn
0.3o
2.Because the effect of three kinds of transition metal in positive electrode is different, in tertiary cathode material, the proportioning of three kinds of metals is different, and the chemical property showing is also different.The chemical property that for example 622 types and 811 type tertiary cathode materials show is exactly that specific capacity is high, but its rate of decay is very fast.And the performance that 333 types and 523 type tertiary cathode materials show is exactly that specific capacity, cycle performance and security performance are all better.Therefore develop better 333 types and 523 type tertiary cathode material synthetic methods are necessary.
Summary of the invention
Technical problem to be solved by this invention is: based on the existing problem of this area synthesis of ternary material, propose a kind of preparation method of ternary material.The object of the present invention is to provide a kind of preparation method of tertiary cathode material, it is by plasma high-temperature fusion, rapidly synthesis of ternary positive electrode by batching.
The technical scheme that realizes the object of the invention is:
A preparation method for ternary cathode material of lithium ion battery, comprises step:
1) compound of nickel salt, cobalt salt, manganese salt, lithium is by nickel: cobalt: manganese: lithium stoichiometric proportion 2-6:2-3:2-4:1 mixes;
2) with alcohol, be abrasive media, step 1) gained mixture is ground 2～8 hours
3) step 2) mixture after grinding is through 100～120 ℃, and drying and processing under 0.009-0.012MPa vacuum degree, dries 6～12 hours, obtains reaction powder;
4) reaction powder is imposed to the plasma-arc of voltage 1～50,000 V, make to react powder melting;
5) frit reaction powder is spurted in cooling device (temperature in cooling chamber is normal temperature) with oxidizing gas, cooling by 2～10 seconds, particle can enter cooling device below by freely falling body, forms the fine particle of ball-type.
Wherein said alcohol is absolute alcohol.
Technical solution of the present invention can utilize existing plasma spraying equipment to complete, for example ZB-80 type or DH-1080 type, DH-X2 type.Plasma high-temperature fusion technology, it is a kind of new technique that development in recent years is got up, principle is: after vacuum system preset vacuum, in melt chamber and cooling chamber, introduce plasma working gas and (be generally inert gas, inert gas is helium, one or more in neon and argon gas, inert gas in melt chamber and cooling chamber can be same, also can be mist), between the two poles of the earth, add voltage, inert gas plasma moment intensification in melt chamber, temperature can reach several thousand degree, can make to add the powder in feed appliance to reach rapidly molten condition, plasma high-speed motion, between particle, can there is sharp impacts, the instant material generating under needed molten condition, by injected gas out, take melt chamber out of, enter in cooling chamber, after cooling, obtain required tertiary cathode material.Due to extreme temperatures, this method can make ternary material form in moment.And can form serialization production.
Reaction powder is put into the feed appliance of plasma spraying equipment, give between plasma spraying equipment the two poles of the earth and add 1～50,000 V voltage, gas plasma in melt chamber is known from experience intensification rapidly in signa, reach several thousand degree, powder is the rapid melting of meeting under the condition of high temperature, plasma high-speed motion, being blended in can sharp impacts, the rapidly required ternary material of generation between the particle in plasma.
Wherein, described nickel salt, cobalt salt, manganese salt are oxalates; The compound of described lithium is lithium hydroxide or lithium carbonate.
Wherein, described step 2) in, the part by weight of alcohol and mixture is 1～10:1.
Wherein, the plasma electric arc current 400-800A in described step 4).
Wherein, the oxidizing gas in described step 5) is the mixture of oxygen, air or oxygen and air.The air oxygen gaseous mixture of preferred oxygen volume ratio 50%.In described step 5), the length of cooling device is 5～10 meters, and cooling device is the closed cavity that is full of air, and in closed cavity, temperature is normal temperature.
Wherein, the nozzle diameter 0.5-10mm for spraying in described step 5).Reinforced speed is 1～100g/s.
Described preparation method, also comprises the step that the cooled particle of described step 5) is pulverized, sieved, 1～20 micron of the granular size that screening obtains.
Beneficial effect of the present invention is:
The preparation method of the ternary material that the present invention proposes, not only can the more convenient positive electrode of synthesis of ternary efficiently, and the ternary material pattern simultaneously obtaining rule is highly spherical, stable electrochemical property.The present invention will prepare burden by plasma high-temperature fusion, rapidly synthesis of ternary positive electrode.This method can be more convenient synthetic highly spherical efficiently, and composition is even, the tertiary cathode material of stable performance.
Accompanying drawing explanation
Fig. 1 is the ternary material SEM photo of the spherical morphology that makes of embodiment 1.
Embodiment
Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention.
Plasma spraying equipment is used the DH-X2 Supersonic Plasma Spraying equipment of Shanghai large Hao Ruifa spray coating mechanical Co., Ltd, outside plasma spraying equipment outlet, have a sealing (thering is dustproof effect), be full of the cooling chamber of air at room temperature, length is 8 meters, can make the molten state material of acquisition fully cooling.
Embodiment 1
To obtain 100g (1.1mol) LiNi
0.3co
0.3mn
0.3o
2positive electrode is example, and needed raw material is for analyzing pure nickel oxalate 82.12g (0.33mol), cobalt oxalate 82.20g (0.33mol), manganese oxalate 80.88g (0.33mol), and hydronium(ion) oxidation lithium 46.17g (1.1mol).
Raw material mixes, and adds 500g absolute alcohol, puts into ball mill (ball mill model: BXQM2L, Nanjing Te Lun new instrument Co., Ltd) in, mix 2 hours, the good wet feed of mix grinding, in the vacuum of 0.01MPa, is dried 12 hours at 100 ℃ of temperature, and the reaction powder that obtains mixing is standby.Reaction powder is put in the feed appliance of plasma spraying equipment according to the speed of 1g/s with feeding screw, and then powder is scraped in high temperature (3500 ℃ of temperature) the plasma fusion chamber that adds 10,000 V voltages, plasma gas is purity oxygen.Utilize the high temperature transient heating of high temperature oxidation stability gas plasma, the immediate reaction of reaction powder, forms rapidly LiNi
0.3co
0.3mn
0.3o
2, utilize the nozzle that nozzle diameter is 0.5mm, spurt in the injection cooling chamber of the 8 meters long sealings that are full of air, be frozen into spherical fine particle, obtaining average grain diameter is 5 microns of tertiary cathode powders.
Cooled particle is pulverized, and with 300 object vibrating screens, sieves, and obtains finished particle.Material granule is that standard is spherical, as shown in Figure 1.0.2C specific discharge capacity is 155mAh/g, specific area 2.1m
2/ g.
Comparative example: nickel oxalate 82.12g (0.33mol), cobalt oxalate 82.20g (0.33mol), the manganese oxalate 80.88g (0.33mol) of same ratio, and hydronium(ion) oxidation lithium 46.17g (1.1mol), after ground and mixed, 900 ℃ of roastings 10 hours and sieve after, the material pattern obtaining is elliposoidal, 0.2C specific discharge capacity is 145mAh/g, specific area 7.6m
2/ g.
Embodiment 2
To obtain 50g (0.55mol) LiNi
0.5co
0.2mn
0.3o
2positive electrode is example, needed raw material is for analyzing pure nickel oxalate 68.44g (0.275mol), cobalt oxalate 27.4g (0.11mol), manganese oxalate 40.44g (0.165mol), and the raw material of hydronium(ion) oxidation lithium 20.08g (0.55mol) composition.
Raw material mixes, and then adds 200g absolute alcohol, puts in ball mill and mixes 6 hours, and the good wet feed of mix grinding, in the vacuum of 0.01MPa, is dried 12 hours at 110 ℃ of temperature, and the reaction powder that obtains mixing is standby.Reaction powder is put in the feed appliance of plasma spraying equipment, and then powder is scraped to (intracavity gas: 50% oxygen adds 50% air) in the high-temperature plasma melt chamber adding after voltage, utilize the high temperature transient heating of 50,000 V high temperature air plasmas, charging rate is 100g/s, the immediate reaction of reaction powder, forms rapidly LiNi
0.5co
0.2mn
0.3o
2, utilize the nozzle that nozzle diameter is 10mm, spurt in the injection cooling chamber of the 8 meters long sealings that are full of air, be frozen into spherical fine particle, obtain average grain diameter and be the tertiary cathode powder of 3 microns.
Cooled particle is pulverized, screening, gets the particle that 250 orders sieve.Pattern is that standard is spherical, and 0.2C specific discharge capacity is 166mAh/g.
Embodiment 3
To obtain 100g (1.1mol) LiNi
0.5co
0.2mn
0.3o
2positive electrode is example, needed raw material is for analyzing pure nickel oxalate 136.87g (0.55mol), cobalt oxalate 54.80g (0.22mol), manganese oxalate 80.88g (0.33mol), and the raw material of hydronium(ion) oxidation lithium 46.17g (1.1mol) composition.
Raw material mixes, add 1000g absolute alcohol, put in ball mill and mix 8 hours, by the good wet feed of mix grinding in the vacuum of 0.01MPa, at 120 ℃ of temperature, dry 6 hours, the reaction powder that obtains mixing is standby, reaction powder is put in the feed appliance of plasma spraying equipment, and then powder is scraped in the high-temperature plasma melt chamber adding after voltage, utilize the high temperature transient heating of the high-temperature gas plasma (50% oxygen adds 50% air) of 40,000 V high temperature air plasmas, the immediate reaction of reaction powder, forms rapidly LiNi
0.5co
0.2mn
0.3o
2, charging rate is 50g/S, utilizes the nozzle that nozzle diameter is 3mm, spurts in the injection cooling chamber of the 10 meters long sealings that are full of air, is frozen into spherical fine particle, obtaining average grain diameter is 4 microns of tertiary cathode powders.
Cooled particle is pulverized, screening, gets the particle that 400 orders sieve.Pattern is that standard is spherical, and 0.2C specific discharge capacity is 168mAh/g.
Embodiment 4
To obtain 100g (1.03mol) LiNi
0.6co
0.2mn
0.2o
2positive electrode is example, needed raw material is for analyzing pure nickel oxalate 153.80g (0.618mol), cobalt oxalate 51.31g (0.206mol), manganese oxalate 50.49g (0.206mol), and the raw material of hydronium(ion) oxidation lithium 43.23g (1.03mol) composition.
Raw material mixes, add 500g absolute alcohol, put in ball mill and mix 8 hours, by the good wet feed of mix grinding in the vacuum of 0.01MPa, at 120 ℃ of temperature, dry 8 hours, the reaction powder that obtains mixing is standby, reaction powder is put in the feed appliance of plasma spraying equipment, and then powder is scraped in the high-temperature plasma melt chamber adding after voltage, utilize the high temperature transient heating of the high temperature air plasma of 3.5 ten thousand V high temperature air plasmas, the immediate reaction of reaction powder, forms rapidly LiNi
0.6co
0.2mn
0.2o
2, charging rate is 20g/S, utilizes the nozzle that nozzle diameter is 2mm, spurts in the injection cooling chamber of the 15 meters long sealings that are full of air, is frozen into spherical fine particle, obtaining average grain diameter is 3.5 microns of tertiary cathode powders.
Cooled particle is pulverized, screening, gets 350 object particles and observes and measure.Pattern is that standard is spherical, and 0.2C specific discharge capacity is 175mAh/g.
Above embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not departing from the present invention; various modification and improvement that the common engineers and technicians in this area make technical scheme of the present invention, all should fall in the definite protection range of claims of the present invention.
Claims (9)
1. a preparation method for ternary cathode material of lithium ion battery, comprises step:
1) compound of nickel salt, cobalt salt, manganese salt, lithium is by nickel: cobalt: manganese: lithium stoichiometric proportion 2～6:2～3:2～4:1 mixes;
2) with alcohol, be abrasive media, step 1) gained mixture is ground 2～8 hours;
3) step 2) mixture after grinding is through 100～120 ℃, and drying and processing under 0.009～0.012MPa vacuum degree, dries 6～12 hours, obtains reaction powder;
4) reaction powder is imposed to the plasma-arc of voltage 1～50,000 V, make to react powder melting;
5) frit reaction powder is spurted in cooling device with oxidizing gas, cooling by 2～10 seconds, particle can enter cooling device below by freely falling body, forms the fine particle of ball-type.
2. preparation method according to claim 1, is characterized in that, described nickel salt, cobalt salt, manganese salt are oxalates; The compound of described lithium is lithium hydroxide or lithium carbonate.
3. preparation method according to claim 1, is characterized in that, described step 2) in, the part by weight of alcohol and mixture is 1～10:1.
4. preparation method according to claim 1, is characterized in that, the plasma electric arc current 400～800A in described step 4).
5. preparation method according to claim 1, is characterized in that, the nozzle diameter 0.5～10mm for spraying in described step 5).
6. preparation method according to claim 1, is characterized in that, the oxidizing gas in described step 5) is the mixture of oxygen, air or oxygen and air.
7. according to the arbitrary described preparation method of claim 1～6, it is characterized in that, in described step 5), the length of cooling device is 5～10 meters, and cooling device is the closed cavity that is full of air, and in closed cavity, temperature is normal temperature.
8. according to the arbitrary described preparation method of claim 1～6, it is characterized in that, in described step 5), the speed of frit reaction powder feed is 1～100g/s.
9. according to the arbitrary described preparation method of claim 1～6, it is characterized in that, also comprise the step that the cooled particle of described step 5) is pulverized, sieved, the granular size that screening obtains is 1～20 micron.
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| XIAOFENG ZHANG AND RICHARD L.AXELBAUM: "Spray Pyrolysis Synthesis of Mesoporous Lithium-Nickel-Manganese-Oxides for High Energy Li-Ion Batteries", 《JOURNAL OF THE ELECTROCHEMICAL SOCIETY》, vol. 159, no. 6, 13 April 2012 (2012-04-13), pages 834 - 842, XP055037267, DOI: 10.1149/2.079206jes * |
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