CN103280579B - A kind of high performance lithium ion battery anode material lithium ferric manganese phosphate and preparation method thereof - Google Patents
A kind of high performance lithium ion battery anode material lithium ferric manganese phosphate and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high performance lithium ion battery anode material lithium ferric manganese phosphate and preparation method thereof.The chemical general formula of anode material of lithium battery lithium ferric manganese phosphate is Li1-xMgxFeyMnzPO4, wherein 0 < x≤0.1,0 < y≤0.5,0.95 < y+z < 1.The preparation method of positive pole material phosphoric acid ferrimanganic lithium mainly includes the steps such as raw iron oxide material refines and prepared by activation, presoma, pre-burning, coarse pulverization, sintering；Lithium ferric manganese phosphate material disclosed by the invention and preparation method thereof have preparation the prices of raw materials are cheap, security performance good, preparation technology is simple, material and preparation process environmentally friendly, lithium ion battery positive pole material phosphoric acid ferrimanganic lithium 0.1C multiplying power head prepared is put capacity and is up to 153.8mAh/g, 0.2C multiplying power discharging capacity is more than 140mAh/g, showing good chemical property and high rate performance, the property indices of material has taken into account processing characteristics simultaneously.
Description
Technical field
The present invention relates to a kind of high performance lithium ion battery anode material lithium ferric manganese phosphate and preparation method thereof, belong to technical field of lithium ion.
Background technology
Owing to lithium ion battery has good combination property performance so that it is be widely used in portable energy-storing instrument, particularly both at home and abroad extensive concern and the new-energy automobile industry of research.Anode material for lithium-ion batteries is one of big main raw material(s) of lithium battery four, the anode material for lithium-ion batteries having been commercialized such as cobalt acid lithium, LiMn2O4 and LiFePO4 etc..Although at present cobalt acid lithium material commercialization is the most highly developed, but its selling at exorbitant prices, toxicity compared with big, cobalt resource is limited；The material gram volume of LiMn2O4 is relatively low, high-temperature cycle life is poor.
Olivine-type LiFePO 4 material has theoretical gram volume higher (170mAh/g), the higher (3.4V of running voltage, lithium metal is negative pole), have extended cycle life, the advantage such as good high temperature and security performance, the prices of raw materials are cheap, make this material accelerate in industrialization recent years speed, be widely used in lithium-ion-power cell.
But the running voltage of lithium iron phosphate dynamic battery does not still meets people's requirement to electrokinetic cell high-energy-density density at present, the anode material for lithium-ion batteries of the most more high working voltage is always the direction that research worker is paid close attention to, such as rich lithium mangaic acid, high pressure spinel-type nickel ion doped etc., but above-mentioned high working voltage material tests initial stage also in research and development in current lithium battery industrial system.
Vast research worker carries out improving the improvement experiment of material specific energy on the basis of LiFePO 4 material, as CN101997118A discloses a kind of lithium ion battery positive pole material phosphoric acid ferrimanganic lithium and preparation method thereof, consisting of Li1- yMyFe1-xMnxPO4, one or more during wherein M is Mo, Mg, Zn, V, W, Ru, 0.4 ＜ x≤0.7,0.01≤y≤0.1, the lithium ferric manganese phosphate positive electrode 0.1C discharge capacity that this invention prepares reaches 138mAh/g, and the specific energy of material reaches 522.5Wh/kg.The lithium ferric manganese phosphate positive electrode 0.1C discharge capacity utilizing the technology of the present invention to synthesize is up to 153.8mAh/g, and material specific energy reaches 545.7Wh/kg, and material property has substantially had further lifting.
Summary of the invention
It is an object of the invention to provide a kind of high performance lithium ion battery anode material lithium ferric manganese phosphate and system thereof
Preparation Method, compared with LiFePO 4 material, improves the running voltage of synthetic material and the specific energy of material, thus the specific energy density of beneficially later stage battery core promotes.
The technical solution used in the present invention is as follows:
The chemical general formula of a kind of high performance lithium ion battery anode material lithium ferric manganese phosphate is Li1-xMgxFeyMnzPO4, wherein 0 < x≤0.1,0 < y≤0.5,0.95 < y+z < 1.By reducing positive electrode Li1-xMgxFeyMnzPO4Middle Fe, Mn metal element content, can reduce positive electrode Fe element in electrical property cyclic process and separate out and the dissolving of Mn element.
A kind of preparation method of high performance lithium ion battery anode material lithium ferric manganese phosphate, concrete step of preparation process is as follows:
(1) raw iron oxide material refinement and activation: with carbon source 1:0.2-0.6 in mass ratio, micron ferric oxide raw material is carried out dispensing, carries out ball milling 1-5h in organic solvent system, is adjusted activated sintering after drying in controllable type atmosphere furnace and processes；Activated sintering concretely comprises the following steps: activation heat preservation zone is 500-800 DEG C; room temperature heats up to activation heat preservation zone with 2-5 DEG C/min; heat preservation zone temperature retention time is 2-6h, is changed sintering atmosphere into oxygen protection by nitrogen protection, obtain active oxidation iron material after being cooled to room temperature at the end of insulation；
(2) precursor synthesis: by lithium source, magnesium source, active oxidation iron material, manganese source, phosphorus source, carbon source by certain mole of stoichiometric coefficient proportioning, grinds refinement 2-5h under organic solvent system, remains pre-burning through dried presoma mixed powder；
(3) pre-burning: dried presoma mixed powder, in the range of 2-5 DEG C/min, is incubated 2-10h and 1-3h between 350-450 DEG C and 550-650 DEG C of warm area, is cooled to room temperature with body of heater by control heating rate under nitrogen protection respectively, obtains carbon cladding presoma；
(4) coarse pulverization: the carbon after pre-burning is coated with presoma and carries out coarse pulverization process, after controlling coarse pulverization, carbon is coated with the granularity D100 ＜ 100um of presoma；
(5) sintering: under nitrogen protection, control heating rate to be 2-5 DEG C/min by the carbon through coarse pulverization be coated with presoma as 650-750 DEG C at sinter, be incubated 5-15h, be cooled to room temperature, prepare carbon cladding lithium ferric manganese phosphate positive electrode.
Described lithium source is one or more in lithium carbonate, lithium acetate, lithium oxalate, Lithium hydrate, lithium dihydrogen phosphate.
Described magnesium source is magnesium acetate.
Described manganese source is one or more in manganese carbonate, manganese oxalate, manganese acetate, manganese dioxide, manganese sesquioxide managnic oxide.
Described phosphorus source is one or more in lithium dihydrogen phosphate, ammonium phosphate, ammonium dihydrogen phosphate, diammonium phosphate.
Carbon source described in step (1) and step (2) is one or more in sucrose, glucose, polyvinyl alcohol, soluble starch, citric acid, phenolic resin, polypropylene, graphite, white carbon black, acetylene black.
Organic solvent system described in step (1) and step (2) is ethanol or acetone system.
Owing to lithium ion battery anode material lithium iron phosphate stain can occur after circulating through long-time chemical property on barrier film, the highest by tenor at stain on barrier film knowable to test, main cause is to occur in that the phenomenon that metallic element deposits at stain, for effectively reducing the appearance of above-mentioned phenomenon, improve the real work voltage of material simultaneously and reduce manganese element meltage in the electrolytic solution, the invention provides a kind of lithium ion battery positive pole material phosphoric acid ferrimanganic lithium and preparation method thereof.
Lithium ferric manganese phosphate material disclosed by the invention and preparation method thereof have preparation the prices of raw materials are cheap, security performance good, preparation technology is simple, material and preparation process environmentally friendly, lithium ion battery positive pole material phosphoric acid ferrimanganic lithium 0.1C multiplying power head prepared is put capacity and is up to 153.8mAh/g, 0.2C multiplying power discharging capacity is more than 140mAh/g, showing good chemical property and high rate performance, the property indices of material has taken into account processing characteristics simultaneously.
Accompanying drawing explanation
Fig. 1 is the XRD figure of carbon cladding lithium ferric manganese phosphate material as prepared by embodiment 1.
Fig. 2 is the 0.1C first charge-discharge curve of carbon cladding lithium ferric manganese phosphate material as prepared by embodiment 1.
Fig. 3 is 0.1C5 circulation discharge curve of carbon cladding lithium ferric manganese phosphate material as prepared by embodiment 1.
Fig. 4 is that the 0.1C of carbon cladding lithium ferric manganese phosphate material fills-0.2C discharge curve as prepared by embodiment 1.
Fig. 5 is the SEM figure of carbon cladding lithium ferric manganese phosphate material as prepared by embodiment 1.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is specifically described, but is not limited only to this.
Embodiment 1
A kind of lithium ion battery positive pole material phosphoric acid ferrimanganic lithium Li0.95Mg0.05Fe0.54Mn0.45PO4Preparation method, its preparation process is as follows:
Raw iron oxide material refinement and activation: micron ferric oxide raw material is carried out dispensing with carbon source 1:0.5 in mass ratio; ball milling 3h in dehydrated alcohol system; dried powder is the most under nitrogen protection; 600 DEG C are risen to from room temperature with 2 DEG C/min speed; after insulation 4h; change protective atmosphere is oxygen, obtains active oxidation iron material after being cooled to room temperature.
Lithium ferric manganese phosphate Li0.95Mg0.05Fe0.54Mn0.45PO4Synthesis: weigh LITHIUM BATTERY Li respectively2CO3350.98g, chemical pure C4H6O4Mg·4H2O107.23g, active oxidation iron material 431.18g, LITHIUM BATTERY NH4H2PO41150.3g, analytical pure MnC2O4·2H2O1102.905g, the sucrose of raw material gross mass 4.5%.Being placed in by above-mentioned raw materials in the mixer grinder that effective cavity is 10L, add 4600mL dehydrated alcohol, agitation grinding 2h, the D50 controlling ground slurry obtains presoma xeraphium less than 2.5um, slurry after being vacuum dried.Presoma xeraphium is placed in the tube furnace of nitrogen protection, is that 2 DEG C/min rises to 400 DEG C from room temperature by heating rate, 400 DEG C of insulation 3h, then rise to 650 DEG C by the programming rate of 2 DEG C/min, be incubated 1h, be cooled to room temperature with body of heater, obtain carbon cladding presoma.Carbon being coated with presoma and carries out coarse pulverization, after controlling coarse pulverization, powder particles D100 is less than 100um.After coarse pulverization, powder is sintered under nitrogen protection, is that 2 DEG C/min rises to 710 DEG C from room temperature with heating rate, is incubated 8h, is cooled to room temperature, prepares carbon cladding lithium ferric manganese phosphate positive electrode.Gained sample has following physical performance after tested: carbon content 1.8%, specific surface area 15.92m2/g；Sample is made the half-cell with lithium metal as negative pole and is tested its electrochemistry capacitance, and 0.1C multiplying power discharge capacity first is 153.8mAh/g, and electric discharge mean voltage is 3.5482V；0.2C multiplying power discharging capacity is 147.2mAh/g, and electric discharge mean voltage is 3.5437V, and material list reveals good high rate performance.
Embodiment 2
A kind of lithium ion battery positive pole material phosphoric acid ferrimanganic lithium Li0.9Mg0.1Fe0.49Mn0.5PO4Preparation method, its preparation process is as follows:
Raw iron oxide material refinement and activation: micron ferric oxide raw material is carried out dispensing with carbon source 1:0.2 in mass ratio; ball milling 2h in dehydrated alcohol system; dried powder is the most under nitrogen protection; 550 DEG C are risen to from room temperature with 2 DEG C/min speed; after insulation 2h; change protective atmosphere is oxygen, obtains active oxidation iron material after being cooled to room temperature.
Lithium ferric manganese phosphate Li0.9Mg0.1Fe0.49Mn0.5PO4Synthesis: weigh LITHIUM BATTERY Li respectively2CO3332.505g, chemical pure C4H6O4Mg·4H2O214.46g, active oxidation iron material 391.26g, LITHIUM BATTERY NH4H2PO41150.3g, analytical pure MnC2O4·2H2O1225.45g, the glucose of raw material gross mass 4.5%.Being placed in by above-mentioned raw materials in the mixer grinder that effective cavity is 10L, add 4600mL dehydrated alcohol, agitation grinding 3h, the D50 controlling ground slurry obtains presoma xeraphium less than 2.5um, slurry after being vacuum dried.Presoma xeraphium is placed in the tube furnace of nitrogen protection, is that 2 DEG C/min rises to 450 DEG C from room temperature by heating rate, 450 DEG C of insulation 2h, then rise to 650 DEG C by the programming rate of 2 DEG C/min, be incubated 1h, be cooled to room temperature with body of heater, obtain carbon cladding presoma.Carbon being coated with presoma and carries out coarse pulverization, after controlling coarse pulverization, powder particles D100 is less than 100um.After coarse pulverization, powder is sintered under nitrogen protection, is that 2 DEG C/min rises to 700 DEG C from room temperature with heating rate, is incubated 12h, is cooled to room temperature, prepares carbon cladding lithium ferric manganese phosphate positive electrode.Gained sample has following physical performance after tested: carbon content 1.92%, specific surface area 17.3m2/g；Sample is made the half-cell with lithium metal as negative pole and is tested its electrochemistry capacitance, and 0.1C multiplying power discharge capacity first is 145.1mAh/g, and electric discharge mean voltage is 3.5537V；0.2C multiplying power discharging capacity is 136.9mAh/g, and electric discharge mean voltage is 3.5068V, and material list reveals good high rate performance.
Embodiment 3
A kind of lithium ion battery positive pole material phosphoric acid ferrimanganic lithium Li0.95Mg0.05Fe0.6Mn0.38PO4Preparation method, its preparation process is as follows:
Raw iron oxide material refinement and activation: micron ferric oxide raw material is carried out dispensing with carbon source 1:0.3 in mass ratio; ball milling 4h in dehydrated alcohol system; dried powder is the most under nitrogen protection; 650 DEG C are risen to from room temperature with 2 DEG C/min speed; after insulation 2h; change protective atmosphere is oxygen, obtains active oxidation iron material after being cooled to room temperature.
Lithium ferric manganese phosphate Li0.95Mg0.05Fe0.6Mn0.38PO4Synthesis: weigh LITHIUM BATTERY LiH respectively2PO4987.335g, chemical pure C4H6O4Mg·4H2O107.23g, active oxidation iron material 479.09g, LITHIUM BATTERY MnCO3436.81g, the polyvinyl alcohol of raw material gross mass 3% and the citric acid of 3.5%.Being placed in by above-mentioned raw materials in the mixer grinder that effective cavity is 10L, add 2000mL dehydrated alcohol, agitation grinding 2h, the D50 controlling ground slurry obtains presoma xeraphium less than 2.5um, slurry after being vacuum dried.Presoma xeraphium is placed in the tube furnace of nitrogen protection, is that 2 DEG C/min rises to 450 DEG C from room temperature by heating rate, 450 DEG C of insulation 2h, then rise to 650 DEG C by the programming rate of 2 DEG C/min, be incubated 1h, be cooled to room temperature with body of heater, obtain carbon cladding presoma.Carbon being coated with presoma and carries out coarse pulverization, after controlling coarse pulverization, powder particles D100 is less than 100um.After coarse pulverization, powder is sintered under nitrogen protection, is that 2 DEG C/min rises to 700 DEG C from room temperature with heating rate, is incubated 12h, is cooled to room temperature, prepares carbon cladding lithium ferric manganese phosphate positive electrode.Gained sample has following physical performance after tested: carbon content 1.62%, specific surface area 18.3m2/g；Sample is made the half-cell with lithium metal as negative pole and is tested its electrochemistry capacitance, and 0.1C multiplying power discharge capacity first is 146.6mAh/g, and electric discharge mean voltage is 3.4656V；0.2C multiplying power discharging capacity is 129mAh/g, and electric discharge mean voltage is 3.4567V, and material list reveals good high rate performance.
Claims (7)
1. the preparation method of a high performance lithium ion battery anode material lithium ferric manganese phosphate, it is characterised in that: the chemical general formula of lithium ion battery positive pole material phosphoric acid ferrimanganic lithium is Li1-xMgxFeyMnzPO4, wherein 0 < x≤0.1,0 < y≤0.5,0.95 < y+z < 1；
Its concrete step of preparation process is as follows:
(1) raw iron oxide material refinement and activation: with carbon source 1:0.2-0.6 in mass ratio, micron ferric oxide raw material is carried out dispensing, carries out ball milling 1-5h in organic solvent system, is adjusted activated sintering after drying in controllable type atmosphere furnace and processes；Activated sintering concretely comprises the following steps: activation heat preservation zone is 500-800 DEG C; room temperature heats up to activation heat preservation zone with 2-5 DEG C/min; heat preservation zone temperature retention time is 2-6h, is changed sintering atmosphere into oxygen protection by nitrogen protection, obtain active oxidation iron material after being cooled to room temperature at the end of insulation；
(2) precursor synthesis: by lithium source, magnesium source, active oxidation iron material, manganese source, phosphorus source, carbon source by certain mole of stoichiometric coefficient proportioning, grinds refinement 2-5h under organic solvent system, remains pre-burning through dried presoma mixed powder；
(3) pre-burning: dried presoma mixed powder, in the range of 2-5 DEG C/min, is incubated 2-10h and 1-3h between 350-450 DEG C and 550-650 DEG C of warm area, is cooled to room temperature with body of heater by control heating rate under nitrogen protection respectively, obtains carbon cladding presoma；
(4) coarse pulverization: the carbon after pre-burning is coated with presoma and carries out coarse pulverization process, after controlling coarse pulverization, carbon is coated with the granularity D100 ＜ 100um of presoma；
(5) sintering: under nitrogen protection, control heating rate to be 2-5 DEG C/min by the carbon through coarse pulverization be coated with presoma as 650-750 DEG C at sinter, be incubated 5-15h, be cooled to room temperature, prepare carbon cladding lithium ferric manganese phosphate positive electrode.
The preparation method of high performance lithium ion battery anode material lithium ferric manganese phosphate the most according to claim 1, it is characterised in that: described lithium source is one or more in lithium carbonate, lithium acetate, lithium oxalate, Lithium hydrate, lithium dihydrogen phosphate.
The preparation method of high performance lithium ion battery anode material lithium ferric manganese phosphate the most according to claim 1, it is characterised in that: described magnesium source is magnesium acetate.
The preparation method of high performance lithium ion battery anode material lithium ferric manganese phosphate the most according to claim 1, it is characterised in that: described manganese source is one or more in manganese carbonate, manganese oxalate, manganese acetate, manganese dioxide, manganese sesquioxide managnic oxide.
The preparation method of high performance lithium ion battery anode material lithium ferric manganese phosphate the most according to claim 1, it is characterised in that: described phosphorus source is one or more in lithium dihydrogen phosphate, ammonium phosphate, ammonium dihydrogen phosphate, diammonium phosphate.
Its preparation method of high performance lithium ion battery anode material lithium ferric manganese phosphate the most according to claim 1, it is characterised in that: the carbon source described in step (1) and step (2) is one or more in sucrose, glucose, polyvinyl alcohol, soluble starch, citric acid, phenolic resin, polypropylene, graphite, white carbon black, acetylene black.
A kind of high performance lithium ion battery anode material lithium ferric manganese phosphate the most according to claim 1 and preparation method thereof, it is characterised in that: the organic solvent system described in step (1) and step (2) is ethanol or acetone system.
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| CN103840159B (en) * | 2014-03-25 | 2016-11-16 | 厦门钨业股份有限公司 | A kind of lithium ion anode material LiFePO4the synthetic method of/C |
| CN105514423A (en) * | 2014-10-17 | 2016-04-20 | 苏州艾美得新能源材料有限公司 | Preparation method of cathode material, cathode material, and battery |
| CN105236379A (en) * | 2015-10-08 | 2016-01-13 | 绍兴文理学院 | Laboratory preparation method of porous positive material for high-capacity lithium batteries |
| CN105742610B (en) * | 2016-05-04 | 2018-09-18 | 合肥国轩高科动力能源有限公司 | A kind of preparation method of carbon coating lithium ferric manganese phosphate film-type positive electrode |
| CN108923090A (en) * | 2018-05-29 | 2018-11-30 | 深圳市德方纳米科技股份有限公司 | A method of carbon-coated lithium iron manganese phosphate anode material is prepared from waste lithium iron phosphate battery recycling |
| CN111559739A (en) * | 2020-03-30 | 2020-08-21 | 桑顿新能源科技有限公司 | High-rate lithium ferric manganese phosphate composite material, preparation method thereof and lithium ion battery |
| CN111933915A (en) * | 2020-09-14 | 2020-11-13 | 天津斯科兰德科技有限公司 | Lithium iron manganese phosphate positive electrode material and preparation method and application thereof |
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| CN101152961A (en) * | 2007-08-10 | 2008-04-02 | 石家庄百思特电池材料有限公司 | Method of producing lithium iron phosphate with high compacted density and excellent adhesive property |
| CN101997118A (en) * | 2010-11-02 | 2011-03-30 | 天津斯特兰能源科技有限公司 | Lithium ferric manganese phosphate as cathode material of lithium ion battery and preparation method thereof |
| CN102569790A (en) * | 2010-12-30 | 2012-07-11 | 北京当升材料科技股份有限公司 | Lithium iron phosphate material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101152961A (en) * | 2007-08-10 | 2008-04-02 | 石家庄百思特电池材料有限公司 | Method of producing lithium iron phosphate with high compacted density and excellent adhesive property |
| CN101997118A (en) * | 2010-11-02 | 2011-03-30 | 天津斯特兰能源科技有限公司 | Lithium ferric manganese phosphate as cathode material of lithium ion battery and preparation method thereof |
| CN102569790A (en) * | 2010-12-30 | 2012-07-11 | 北京当升材料科技股份有限公司 | Lithium iron phosphate material |
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