CN101800315A - Multielement-doped lithium iron phosphate positive electrode material and preparation method thereof - Google Patents

Multielement-doped lithium iron phosphate positive electrode material and preparation method thereof Download PDF

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CN101800315A
CN101800315A CN201010142529A CN201010142529A CN101800315A CN 101800315 A CN101800315 A CN 101800315A CN 201010142529 A CN201010142529 A CN 201010142529A CN 201010142529 A CN201010142529 A CN 201010142529A CN 101800315 A CN101800315 A CN 101800315A
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positive electrode
multielement
electrode material
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商士波
赛喜雅勒图
李安
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QuFu EV Energy Co Ltd
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    • 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 multielement-doped lithium iron phosphate positive electrode material and a preparation method thereof. The general formula of the multielement-doped lithium iron phosphate positive electrode material is Li1-xAxFe1-y-zNbyMzPO4, wherein x, y and z are more than zero and not more than 0.1. The preparation method comprises the following steps: mixing lithium source, iron source, phosphorus source, compound of A and carbon source, roasting at 400-800 DEG C, then quickly reducing the temperature to room temperature, crushing, grinding to obtain an intermediate, then mixing the intermediate with niobium compound, compound of M and carbon source, roasting at 400-850 DEG C, then quickly reducing the temperature to room temperature, grinding, and grading to obtain the product. The preparation method of the invention can obviously increase the tap density of the material; and the material can have higher specific capacity and volume specific capacity and excellent cycle performance, meanwhile the material is applicable to industrialized stable production and has wide application prospect in the battery positive electrode material field for energy sources.

Description

A kind of multielement-doped lithium iron phosphate positive electrode material and preparation method thereof
Technical field
The present invention relates to a kind of multielement-doped lithium iron phosphate positive electrode material of using as secondary lithium battery commonly used or power source and preparation method thereof, belong to the electrochemical power source technical field of material.
Background technology
Lithium ion battery is the novel green high-power rechargeable battery that occurs early 1990s, numerous advantages such as have that voltage height, energy density are big, good cycle, self discharge are little, memory-less effect, operating temperature range are wide, be widely used in fields such as mobile phone, notebook computer, electric tool, electronic instrument, army's construction machinery, in electric motor car, also have a good application prospect, become the emphasis that competitively research and develop countries in the world at present.Positive electrode is an important component part of lithium ion battery, researches and develops the key point that high performance positive electrode has become the lithium ion battery development.
At first proposed LiFePO in 1997 by J.B.Goodenough etc. 4As the secondary lithium battery positive electrode, battery material research staff in various countries' is to LiFePO subsequently 4Carry out researchs such as ion doping and coating, and obtained certain achievement.LiFePO 4Have cheap, nontoxic, nonhygroscopic, Environmental compatibility is fine, rich in mineral resources, multiple advantages such as capacity is higher, safety and stability.Yet there are three significant disadvantages in LiFePO4: the Fe during (1) is synthetic 2+Easily be oxidized to Fe 3+, be difficult to obtain single-phase LiFePO4; (2) conductivity is low, causes high-rate charge-discharge capability poor, and actual specific capacity is low; (3) bulk density is low, causes volume and capacity ratio low.These three shortcomings have hindered the practical application of this material.Existing research mainly improves the performance of LiFePO4 by following approach: (1) adopts inert atmosphere to protect Fe 2+(2) mix conductive carbon material or conductive metal particle,, improve the electronic conductivity of material perhaps toward LiFePO4 particle surface coated with conductive material with carbon element.(3) mix the small amount of impurities metal ion, as Co 2+, Mg 2+, Mn 2+, Cr 2+, Zr 4+, Ni 3+, Ce 4+Replace a part of Li +And Fe 2+The position, thereby make the LiFePO4 intrinsic semiconductor change n type or p N-type semiconductor N into, significantly improved the electronic conductivity of material.(4) LiFePO4 of synthetic small particle diameter improves the diffusivity of lithium ion, has improved the lithium ion conductivity and the stock utilization of material on apparent.
Yet the shortcoming that the LiFePO4 bulk density is low is subjected to people's ignorance and avoidance always, is not resolved as yet, has hindered the practical application of material.The solid density of cobalt acid lithium is 5.1g/cm 3, the tap density of commodity cobalt acid lithium is generally 2.4-3.0g/cm 3And the solid density of LiFePO4 only is 3.6g/cm 3, itself is just much lower than cobalt acid lithium.For improving conductivity, people mix conductive carbon material, have significantly reduced the bulk density of material again, make the tap density of general carbon dope LiFePO4 have only 1.0g/cm 3So low bulk density makes that the volume and capacity ratio of LiFePO4 is more much lower than the sour lithium of cobalt, and the battery volume of making will be very huge, not only have no advantage and can say, and be difficult to be applied to reality.Therefore, the bulk density of raising LiFePO4 and volume and capacity ratio have the decision meaning to the practicability of LiFePO4.
Summary of the invention
The objective of the invention is the shortcoming that density is not high, conductivity is bad, a kind of multielement-doped lithium iron phosphate positive electrode material and preparation method thereof is provided at the said method existence.LiFePO in the multielement-doped lithium iron phosphate positive electrode material of the present invention 4Lithium position and iron position are doped simultaneously in the lattice, and wherein lithium position alloy is the lanthanide series rare-earth elements compound, and iron position alloy is one or more in niobium and magnesium, aluminium, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, zinc, barium, zirconium, indium, the bismuth element compound.
The objective of the invention is to be achieved through the following technical solutions: a kind of multielement-doped lithium iron phosphate positive electrode material is characterized in that its composition general formula is: Li 1-xA xFe 1-y-zNb yM zPO 4Wherein, mix and represent that with A A represents lanthanide series rare-earth elements in the lithium position, and corresponding to the rare earth lanthanide compound, doping is 0＜x≤0.1; The iron position is doped to Nb and M, and Nb is a niobium, and corresponding to the compound of niobium element, doping is 0＜y≤0.1; M represents one or more in magnesium, aluminium, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, zinc, barium, zirconium, indium, the bismuth element, corresponding to the compound of magnesium, aluminium, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, zinc, barium, zirconium, indium, bismuth element, doping is 0＜z≤0.1.
The preparation method of multielement-doped lithium iron phosphate positive electrode material of the present invention, processing step is:
(1) at first lithium source, source of iron, phosphorus source, lanthanide series rare-earth elements compound (compound of A) and carbon source are mixed 1-8h in high speed inclined grinding batch mixer under the ball-milling medium effect, molal quantity is respectively 0.8≤Li≤1.2,0＜A≤0.1,0.8≤Fe≤1, P=1, carbon source accounts for the 1-20% (wt/wt) of raw material summation, under inertia or protection of reducing atmosphere, through 400-800 ℃ of high-temperature roasting 8-30h, drop to room temperature rapidly with the cooling water jacket, after pulverizing, grinding, obtain intermediate again;
(2) then compound, the compound of M, the carbon source of intermediate and niobium are ground in the batch mixer at the high speed inclined and mix 1-8h under the ball-milling medium effect; its molal quantity is: 0＜Nb≤0.1; 0＜M≤0.1; carbon source accounts for the 1-20% (wt/wt) of intermediate; under inertia or protection of reducing atmosphere; 400-850 ℃ of high-temperature roasting 8-30h drops to room temperature rapidly with the cooling water jacket, obtains target product behind the crushing and classification.
Ball-milling medium of the present invention is one or more in polyurethane ball, zirconia ball, agate ball, alumina balls, the stainless steel ball.
Described inert atmosphere or reducing atmosphere are one or more in nitrogen, argon gas, hydrogen, the argon hydrogen gaseous mixture.Described lithium source is one or more in lithium carbonate, lithium hydroxide, lithium oxalate, the lithium acetate.Described source of iron is one or more in ferrous oxalate, ferrous acetate, ferrous sulfate, ferrous phosphate, ferric phosphate, the di-iron trioxide; Described phosphorus source is that phosphate comprises one or more in ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, the ferric phosphate.Described carbon source is one or more in glucose, sucrose, starch, acetylene black, the carbon black.The compound of described A is one or more in oxide, hydroxide, chloride, nitrate, sulfate, carbonate, fluoride and the organic salt of the lanthanum except that the radioactivity promethium, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium in the lanthanide series.The compound of described niobium is one or both in niobium pentaoxide, the niobium hydroxide.The compound of described M is one or more in oxide, hydroxide, chloride, nitrate, sulfate, carbonate, fluoride and the organic salt of magnesium, aluminium, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, zinc, barium, zirconium, indium, bismuth.
Multielement-doped lithium iron phosphate positive electrode material of the present invention is applied to the preparation technology of lithium battery, its application process is: multielement-doped lithium iron phosphate powder 85-90% (wt/wt) is applied on the collector aluminium foil after grinding evenly with conductive carbon black 5-10% (wt/wt), Kynoar 5%, make positive plate, with the metal lithium sheet is negative pole, with LiPF 6Be dissolved in volume ratio and be in 1: 1 ethyl carbonate and the dimethyl carbonate mixed solvent as electrolyte its LiPF 6Concentration is 1mol/L in electrolyte; Microporous polypropylene membrane is a barrier film, is assembled into simulation secondary lithium-ion rechargeable battery; Carry out constant-current constant-voltage charging, constant-current discharge with the chemical property tester, discharging and recharging cut-ff voltage is 3.0V-4.2V, and discharge-rate charges and discharge for the last fortnight 0.2C, charges and discharge circulation for 1C later on.
The invention has the beneficial effects as follows: utilization of the present invention is easy to the high temperature solid-phase sintering method of suitability for industrialized production, alloy is drawn materials extensively, through simple hybrid technique, do not contain solvent, pollute little, control heat treatment temperature and time by twice high temperature sintering, circulating water cooling is grown up the material granule secondary crystallization, and crystal property is good, composition is even, and tap density can reach 1.5-2.0g/cm 3, first discharge specific capacity can reach 140-160mA/g under the room temperature.Preparation method of the present invention has not only significantly improved the tap density of material, and make material have higher specific capacity, volume and capacity ratio and excellent cycle performance, preparation method of the present invention is applicable to the industrialization steady production simultaneously, has wide application prospect at power source with the cell positive material field.
Description of drawings
Fig. 1 is the electron scanning micrograph of multielement-doped lithium iron phosphate material among the embodiment 1.
Fig. 2 is the multiplying power discharging curve behind the multielement-doped lithium iron phosphate material composition battery among the embodiment 1.
Embodiment
Below with example the method that the present invention prepares multielement-doped lithium iron phosphate positive electrode material is further described, help the present invention is done further understanding.
Embodiment 1:
With pure Lithium Carbonate Li 2CO 3366.3g, cerium oxide CeO 217.2g, ferrous oxalate Fe (C 2O 4) 2H 2O1773g, ammonium dihydrogen phosphate NH 4H 2PO 41150g, glucose 99.2g, adding the high speed inclined grinds in the batch mixer, with the polyurethane ball is ball-milling medium mixing 6h, then under 0.3 liter/minute nitrogen atmosphere, rise to 600 ℃ with 5 ℃/minute heating rates, at this temperature insulation 10h, drop to room temperature rapidly with the cooling water jacket, pulverizing obtains intermediate after grinding.
Add niobium pentaoxide Nb again 2O 513.3 gram, magnesium oxide MgO 2g, glucose 99.2g, grind in the batch mixer at the high speed inclined, with the polyurethane ball is ball-milling medium mixing 6h, then under 0.3 liter/minute nitrogen atmosphere, rise to 800 ℃ with 5 ℃/minute heating rates, at this temperature insulation 18h, drop to room temperature rapidly with the cooling water jacket, pulverizing is ground and obtained composition formula is Li 0.99Ce 0.01Fe 0.985Nb 0.01Mg 0.005PO 4LiFePO 4 powder.Recording the product tap density is 1.6g/cm 3, be that negative pole records this product first discharge specific capacity 154mA/g with the metal lithium sheet under the room temperature, discharge and recharge capability retention 〉=98% 50 times.
Embodiment 2:
With pure Lithium Carbonate Li 2CO 3366.3g, lanthana La 2O 316.3g, ferrous oxalate Fe (C 2O 4) 2H 2O 1764g, diammonium hydrogen phosphate (NH 4) 2HPO 41320g, sucrose 104.1g, adding the high speed inclined grinds in the batch mixer, with the polyurethane ball is ball-milling medium mixing 6h, then under 0.3 liter/minute nitrogen atmosphere, rise to 700 ℃ with 5 ℃/minute heating rates,, drop to room temperature rapidly with the cooling water jacket at this temperature insulation 10h, obtain intermediate after pulverizing grinding, add niobium pentaoxide Nb again 2O 513.3g, magnesium oxide MgO 2g, manganese dioxide MnO 24.35g, glucose 104.1g, grind in the batch mixer at the high speed inclined, with the polyurethane ball is ball-milling medium mixing 6h, then under 0.3 liter/minute nitrogen atmosphere, rise to 800 ℃ with 5 ℃/minute heating rates, at this temperature insulation 18h, drop to room temperature rapidly with the cooling water jacket, pulverizing is ground and obtained composition formula is Li 0.99La 0.01Fe 0.98Nb 0.01Mg 0.005Mn 0.005PO 4LiFePO 4 powder.Recording the product tap density is 1.63g/cm 3, be that negative pole records this product first discharge specific capacity 155mA/g with the metal lithium sheet under the room temperature, discharge and recharge capability retention 〉=99% 50 times.
Embodiment 3:
With pure Lithium Carbonate Li 2CO 3366.3g, lanthana La 2O 316.3g, di-iron trioxide Fe 2O 31568g, ammonium dihydrogen phosphate NH 4H 2PO 41150g, carbon black 310.4g, adding the high speed inclined grinds in the batch mixer, with the polyurethane ball is ball-milling medium mixing 6h, then under 0.3 liter/minute nitrogen atmosphere, rise to 750 ℃ with 5 ℃/minute heating rates,, drop to room temperature rapidly with the cooling water jacket at this temperature insulation 10h, obtain intermediate after pulverizing grinding, add niobium pentaoxide Nb again 2O 513.3g, magnesium oxide MgO 2g, manganese dioxide MnO 24.35g, carbon black 155.2g, grind in the batch mixer at the high speed inclined, with the polyurethane ball is ball-milling medium mixing 6h, then under 0.3 liter/minute nitrogen atmosphere, rise to 800 ℃ with 5 ℃/minute heating rates, at this temperature insulation 18h, drop to room temperature rapidly with the cooling water jacket, pulverizing is ground and obtained composition formula is Li 0.99La 0.01Fe 0.98Nb 0.01Mg 0.005Mn 0.005PO 4LiFePO 4 powder.Recording the product tap density is 1.68g/cm 3, be that negative pole records this product first discharge specific capacity 152mA/g with the metal lithium sheet under the room temperature, discharge and recharge capability retention 〉=99% 50 times.
Embodiment 4
With pure Lithium Carbonate Li 2CO 3366.3g, cerium oxide CeO 217.2g, ferric phosphate FePO 41510g, carbon black 284.6g, adding the high speed inclined grinds in the batch mixer, with the polyurethane ball is ball-milling medium mixing 6h, then under 0.3 liter/minute nitrogen atmosphere, rise to 600 ℃ with 5 ℃/minute heating rates,, drop to room temperature rapidly with the cooling water jacket at this temperature insulation 10h, obtain intermediate after pulverizing grinding, add niobium pentaoxide Nb again 2O 513.3g, magnesium oxide MgO 2g, carbon black 94.9g, grind in the batch mixer at the high speed inclined, with the polyurethane ball is ball-milling medium mixing 6h, then under 0.3 liter/minute nitrogen atmosphere, rise to 850 ℃ with 5 ℃/minute heating rates, at this temperature insulation 18h, drop to room temperature rapidly with the cooling water jacket, pulverizing is ground and obtained composition formula is Li 0.99Ce 0.01Fe 0.985Nb 0.01Mg 0.005PO 4LiFePO 4 powder.Recording the product tap density is 1.70g/cm 3, be that negative pole records this product first discharge specific capacity 148mA/g with the metal lithium sheet under the room temperature, discharge and recharge capability retention 〉=98% 50 times.

Claims (6)

1. a multielement-doped lithium iron phosphate positive electrode material is characterized in that, its composition general formula is: Li 1-xA xFe 1-y-zNb yM zPO 4Wherein, 0＜x≤0.1,0＜y≤0.1,0＜z≤0.1, A represents lanthanide series rare-earth elements, and M represents one or more in magnesium, aluminium, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, zinc, barium, zirconium, indium, the bismuth element.
2. a kind of multielement-doped lithium iron phosphate positive electrode material as claimed in claim 1 is characterized in that, its tap density is 1.5-2.0g/cm 3, first discharge specific capacity is 140-160mA/g under the room temperature.
3. the preparation method of the described multielement-doped lithium iron phosphate positive electrode material of claim 1 is characterized in that, may further comprise the steps:
(1) at first compound and the carbon source of lithium source, source of iron, phosphorus source, A are mixed 1-8h in high speed inclined grinding batch mixer under the ball-milling medium effect, molal quantity is respectively 0.8≤Li≤1.2,0＜A≤0.1,0.8≤Fe≤1, P=1, carbon source is the 1-20% of raw material quality summation, under inertia or protection of reducing atmosphere, through 400-800 ℃ of high-temperature roasting 8-30h, drop to room temperature rapidly with the cooling water jacket, after pulverizing, grinding, obtain intermediate again;
(2) then compound, the compound of M, the carbon source of intermediate and niobium are ground in the batch mixer at the high speed inclined and mix 1-8h under the ball-milling medium effect; its molal quantity is: 0＜Nb≤0.1; 0＜M≤0.1; carbon source is the 1-20% of intermediate quality; under inertia or protection of reducing atmosphere; 400-850 ℃ of high-temperature roasting 8-30h drops to room temperature rapidly with the cooling water jacket, obtains target product behind the crushing and classification.
4. the preparation method of multielement-doped lithium iron phosphate positive electrode material as claimed in claim 3 is characterized in that, described ball-milling medium is one or more in polyurethane ball, zirconia ball, agate ball, alumina balls, the stainless steel ball.
5. the preparation method of multielement-doped lithium iron phosphate positive electrode material as claimed in claim 3 is characterized in that, described inert atmosphere or reducing atmosphere are one or more in nitrogen, argon gas, hydrogen, the argon hydrogen gaseous mixture.
6. as the preparation method of any described multielement-doped lithium iron phosphate positive electrode material among the claim 3-5, it is characterized in that described lithium source is one or more in lithium carbonate, lithium hydroxide, lithium oxalate, the lithium acetate; Described source of iron is one or more in ferrous oxalate, ferrous acetate, ferrous sulfate, ferrous phosphate, ferric phosphate, the di-iron trioxide; Described phosphorus source is that phosphate comprises one or more in ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, the ferric phosphate; Described carbon source is one or more in glucose, sucrose, starch, acetylene black, the carbon black; The compound of described A is one or more in oxide, hydroxide, chloride, nitrate, sulfate, carbonate, fluoride and the organic salt of the lanthanum except that the radioactivity promethium, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium in the lanthanide series; The compound of described niobium is one or both in niobium pentaoxide, the niobium hydroxide; The compound of described M is one or more in oxide, hydroxide, chloride, nitrate, sulfate, carbonate, fluoride and the organic salt of magnesium, aluminium, titanium, vanadium, chromium, manganese, cobalt, nickel, copper, zinc, barium, zirconium, indium, bismuth.
CN201010142529A 2010-04-09 2010-04-09 Multielement-doped lithium iron phosphate positive electrode material and preparation method thereof Pending CN101800315A (en)

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CN102185146A (en) * 2011-03-18 2011-09-14 宁波职业技术学院 Rare-earth doped manganese-lithium phosphate anode material and preparation method thereof
CN102420329A (en) * 2011-10-18 2012-04-18 新乡市中科科技有限公司 High-tap-density composite modified cathode material of lithium ion battery and preparation method thereof
CN102569738A (en) * 2010-12-30 2012-07-11 北京当升材料科技股份有限公司 Preparation method of lithium iron phosphate material
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CN105355859A (en) * 2015-12-21 2016-02-24 宁波高新区锦众信息科技有限公司 Preparation method of magnesium and barium doped lithium iron phosphate cathode material for lithium ion battery
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CN102569738A (en) * 2010-12-30 2012-07-11 北京当升材料科技股份有限公司 Preparation method of lithium iron phosphate material
CN102185146A (en) * 2011-03-18 2011-09-14 宁波职业技术学院 Rare-earth doped manganese-lithium phosphate anode material and preparation method thereof
CN102185146B (en) * 2011-03-18 2013-11-06 宁波职业技术学院 Rare-earth doped manganese-lithium phosphate anode material and preparation method thereof
CN102420329B (en) * 2011-10-18 2014-10-29 新乡市中科科技有限公司 High-tap-density composite modified cathode material of lithium ion battery and preparation method thereof
CN102420329A (en) * 2011-10-18 2012-04-18 新乡市中科科技有限公司 High-tap-density composite modified cathode material of lithium ion battery and preparation method thereof
CN102730660A (en) * 2012-06-06 2012-10-17 韦丽梅 Preparation method of europium doped barium iron phosphate
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Application publication date: 20100811