CN101058440A - Preparation of positive electrode material Li(1+x)V3O8 of lithium ion cell and doping method - Google Patents

Preparation of positive electrode material Li(1+x)V3O8 of lithium ion cell and doping method Download PDF

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CN101058440A
CN101058440A CNA2007100197486A CN200710019748A CN101058440A CN 101058440 A CN101058440 A CN 101058440A CN A2007100197486 A CNA2007100197486 A CN A2007100197486A CN 200710019748 A CN200710019748 A CN 200710019748A CN 101058440 A CN101058440 A CN 101058440A
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glycine
lithium
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mol ratio
deionized water
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CN100480189C (en
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鲁道荣
李枝贤
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Hefei University of Technology
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Hefei University of Technology
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    • Y02E60/10—Energy storage using batteries

Abstract

The invention discloses a making method of lithium ion battery anode material Li1+xV3O8, which comprises the following steps: adopting lithium hydroxide and ammonium metavanadate as raw material; using glycine as complexing agent; setting the molar rate of lithium and vanadium at 0. 90-1. 15/3 and the molar rate of vanadium and glycine at 1. 0/1. 2-1. 8; blending evenly to dissolve in the deionized water; stirring under 70-85 deg. c until dissolving completely; heating on the electric stove to react; evaporating to obtain the predecessor; grinding the predecessor at 8-15deg. c/min; heating to 420-450 deg. c for 18-22h; cooling to obtain the product. The doping method of Li1+xV3O8 comprises the following steps: blending cobaltous carbonate, nickel carbonate and lithium hydroxide, ammonium metavanadate and glycine in the deionized water; stirring under 70-80 deg. c to disperse evenly; heating to react; evaporating; sintering; obtaining Li1+xCoyV3-yO8 and Li1+xCoyNiyV3-2yO8 as anode material. The method simplifies the technical flow path to shorten the reacting time, which improves the specific capacity of battery and pressure of the discharge platform with good circulating property.

Description

Anode material for lithium-ion batteries Li 1+xV 3O 8Preparation and adulterating method
One, technical field
The present invention relates to a kind of preparation method of chemical power source electrode materials, particularly the preparation method of lithium ion battery electrode material exactly is a kind of anode material for lithium-ion batteries Li 1+xV 3O 8, Li 1+xCo yV 3-yO 8And Li 1+xCo yNi yV 3-2yO 8The preparation method.
Two, background technology
Anode material for lithium-ion batteries Li with laminate structure 1+xV 3O 8, big because of its specific storage, have extended cycle life, have good embedding lithium ability, and can overcome shortcomings such as deep discharge that two chalcogenides can not bear and moisture-sensitive, thereby become one of cell positive material that people are concerned about.
At present, the report for preparing this positive electrode material is more, and solid phase method is arranged, hydrothermal method, the precipitator method, sol-gel method etc.Wherein, most of report all adopts sol-gel method.But the report of relevant this positive electrode material preparation all is to make complexing agent with citric acid, begins to solution concentration, drying, roasting from reaction, need the process of a complexity, and the time is longer, is unfavorable for industrialization.Simultaneously, resulting product particle is bigger, and size distribution neither be very even.And the specific storage of prepared material is also undesirable.Therefore, be necessary to develop the positive electrode material Li that a kind of preparation method is simple, can be applicable to suitability for industrialized production and specific storage height, good cycle 1+xV 3O 8Novel method.
Three, summary of the invention
Preparation anode material for lithium-ion batteries Li provided by the invention 1+xV 3O 8And pass through Li 1+xV 3O 8Preparation Li mixes 1+xCo yV 3-yO 8And Li 1+xCo yNi yV 3-2yO 8Novel method, be intended to simplify reaction process, shorten the reaction times, improve specific storage, discharge platform voltage and the thermostability of product simultaneously, improve its cycle performance.Technical problem to be solved is to select new complexing agent and preparation technology.
Positive electrode material Li 1+xV 3O 8The preparation method be to be raw material with lithium hydroxide, ammonium meta-vanadate, comprise mixing, reaction, evaporate to dryness, roasting and cooling, difference with the prior art is: the selection glycine is a complexing agent, concrete grammar is to get lithium hydroxide (LiOH), ammonium meta-vanadate (NH 4VO 3) and glycine (C 2H 5O 2N) mixing is dissolved in the deionized water, under 70～85 ℃ of conditions, be stirred to dissolving fully, make it to mix, reacting by heating and evaporate to dryness obtain presoma on the 800w electric furnace then, at last presoma is ground the back and be warming up to 420～450 ℃, and 18～22 hours postcooling of constant temperature calcining promptly get anode material for lithium-ion batteries Li with 8～15 ℃/min speed 1+xV 3O 8Lithium/vanadium during mixing (Li/V) mol ratio is 0.90～1.15/3, vanadium/glycine (V/C 2H 5O 2N) mol ratio is 1.0/1.2～1.8.
Preferably: the Li/V mol ratio is 1.05/3, V/C 2H 5O 2The N mol ratio is 1.0/1.5.
The concrete operations step is as follows:
(1) accurately takes by weighing a certain amount of LiOHH by a certain percentage 2O, NH 4VO 3And C 2H 5O 2N mixes in beaker.
(2) said mixture is dissolved in the deionized water, under 70～85 ℃, carries out earlier magnetic agitation 0.4～0.8h, form homogeneous system.
(3) homogeneous system in the step 2 is poured in the crucible, be placed on the 800W pressure regulation electrothermal oven and heat, behind reaction and the evaporate to dryness, obtain presoma.
(4) presoma is ground be placed in the chamber type electric resistance furnace, be warming up to 420～450 ℃ temperature and constant temperature calcining 18～22h, promptly obtain positive electrode material Li behind the naturally cooling with 8～15 ℃/min speed 1+xV 3O 8
Anode material for lithium-ion batteries Li 1+xCo yV 3-yO 8And Li 1+xCo yNi yV 3-2yO 8The preparation method be exactly at above preparation Li 1+xV 3O 3Carry out adulterated method in the process, concrete grammar is to add a certain proportion of cobaltous carbonate (2CoCO when mixing 33Co (OH) 2XH 2O) and nickelous carbonate (NiCO 32Ni (OH) 24H 2O) one dispersed with stirring is even, and later operation steps is identical.Promptly obtain positive electrode material Li 1+xCo yV 3-yO 8(monobasic doping) and Li 1+xCo yNi yV 3-2yO 8(binary doped).
Described certain proportion is: the Li/Co mol ratio is that 1.0/0.01～0.05, Li/Ni mol ratio are 1.0/0.01～0.05, and Co and Ni mol ratio are 1.0/1.0 (binary doped).
The described heating on electrothermal oven is: the output terminal of voltate regulator is connected with electrothermal oven, is 180～220V by regulating voltage.
Described roasting method is: 8～15 ℃/min of temperature rise rate, and 420～450 ℃ of maturing temperatures, roasting time is 20～24h.
The glycine of selecting for use proposed by the invention is the preparation anode material for lithium-ion batteries Li of complexing agent 1+xV 3O 8And the method for doping Co and Ni has the following advantages: this method has not only shortened the reaction times, has simplified reaction process, and prepared powder exquisiteness, has good flowability, and key is that (discharging current is 5mA/g to the specific storage that has improved battery Active substanceThe time, specific storage reaches 400mAh/g) and the voltage (than about the high 0.05V of bibliographical information value) of discharge platform, and good cycle is (with 5mA/g Active substanceDischarge, 40 circulation back capacity attenuations 6%; With 10mA/g Active substanceDischarge, 40 circulation back capacity attenuations 11%).Simultaneously, facility investment is less, is convenient to suitability for industrialized production.
Four, description of drawings
Fig. 1 is the anode material for lithium-ion batteries Li that the present invention prepares 1+xV 3O 8X-ray diffractogram, adopt the Japanese D/Max-rB of company type X-ray diffractometer of science (pipe is pressed 40.0KV, tube current 0.100A, 6 °/min of scanning speed, 10～65 ° of sweep limits for Cu target, K α=0.1541nm).Wherein the position of each crystal face diffraction peak is similar to JCPDS card (72-1193) with relative intensity, shows that products therefrom is positive electrode material LiV 3O 8
Fig. 2 is the anode material for lithium-ion batteries Li that the present invention prepares 1+xV 3O 8TEM figure, the product particle be a bulk, globule size is more even.
Fig. 3 is binary doped anode material for lithium-ion batteries Li 1+xCo yNi yV 3-2yO 8Cycle performance figure.Loading capacity is 390mAh/g first, and 20 times circulation back capacity attenuation is 4% (discharging current 6mA/g active substance).
Five, embodiment
(1) Li 1+xV 3O 8Preparation
Embodiment 1:
With 0.0105mol LiOHH 2O, 0.03mol NH 4VO 3With 0.045mol C 2H 5O 2N mixes in beaker, adds deionized water and is diluted to 300ml.Then said mixture is carried out magnetic agitation 0.5h under 80 ℃, make it to form homogeneous system.This homogeneous system is poured in the crucible, be placed on reacting by heating on the 800W electric furnace, by regulating the voltate regulator be connected with electric furnace, control voltage is 200V, treat the water evaporate to dryness after, obtain presoma.Presoma ground be placed in the chamber type electric resistance furnace, be warming up to 420 ℃ with the temperature rise rate of 10 ℃/min, and, promptly obtain positive electrode material Li behind the naturally cooling at this roasting temperature 20h 1+xV 3O 8
Embodiment 2:
With 0.0105mol LiOHH 2O, 0.03mol NH 4VO 3With 0.036mol C 2H 5O 2N mixes in beaker, adds deionized water and is diluted to 350ml.Then said mixture is carried out magnetic agitation 0.4h under 85 ℃, make it to form homogeneous system.This homogeneous system is poured in the crucible, be placed on reacting by heating on the 800W electrothermal oven, by regulating the voltate regulator that is connected with electrothermal oven, control voltage is 220V.After treating the water evaporate to dryness, obtain presoma.Presoma ground be placed in the chamber type electric resistance furnace, be warming up to 440 ℃ with the temperature rise rate of 8 ℃/min, and, promptly obtain positive electrode material Li behind the naturally cooling at this roasting temperature 22h 1+xV 3O 8
Embodiment 3:
With 0.0105mol LiOHH 2O, 0.0298mol NH 4VO 3, 0.048mol C 2H 5O 2N and mixing in beaker adds deionized water and is diluted to 320ml.Then said mixture is carried out magnetic agitation 0.75h under 75 ℃, make it to form homogeneous system.This homogeneous system is poured in the crucible, be placed on reacting by heating on the 800W electrothermal oven, by regulating the voltate regulator that is connected with electrothermal oven, control voltage is 180V.After treating the water evaporate to dryness, obtain presoma.Presoma ground be placed in the chamber type electric resistance furnace, be warming up to 450 ℃ with the temperature rise rate of 15 ℃/min, and, promptly obtain positive electrode material Li behind the naturally cooling at this roasting temperature 18h 1+xV 3O 8
Embodiment 4:
With 0.0105mol LiOHH 2O, 0.0298mol NH 4VO 3With 0.054mol C 2H 5O 2N mixes in beaker, adds deionized water and is diluted to 400ml.Then said mixture is carried out magnetic agitation 0.8h under 80 ℃, make it to form homogeneous system.This homogeneous system is poured in the crucible, be placed on reacting by heating on the 800W electrothermal oven, by regulating the voltate regulator that is connected with electrothermal oven, control voltage is 190V.After treating the water evaporate to dryness, obtain presoma.Presoma ground be placed in the chamber type electric resistance furnace, be warming up to 430 ℃ with the temperature rise rate of 12 ℃/min, and, promptly obtain positive electrode material Li behind the naturally cooling at this roasting temperature 20h 1+xV 3O 8
(2) Li 1+xCo yV 3-yO 8Preparation
In above example 1～4, get 2CoCO 33Co (OH) 2XH 2The LiOHH of O and metering 2O, NH 4VO 3And C 2H 5NO 2Mix in beaker together, add deionized water and be diluted to 300～400ml, in 70～85 ℃ of magnetic agitation 0.4-0.8h, make it to form homogeneous system, later operation is identical.
Embodiment 5:
With 1.05 * 10 -2Mol LiOHH 2O, 2.98 * 10 -2MolNH 4VO 3, 4.47 * 10 -2Mol C 2H 5O 2N and 2.0 * 10 -5Mol2CoCO 33Co (OH) 2XH 2O mixes in beaker, is diluted to 300ml with deionized water.This mixture is carried out magnetic agitation 0.4h under 80 ℃, make it to form homogeneous system.Be poured in the crucible then, be placed on reacting by heating on the 800W electrothermal oven, by regulating voltage is 200V, after forming the xerogel presoma, this presoma ground be placed in the chamber type electric resistance furnace, be warming up to 420 ℃, constant temperature calcining 20h with the temperature rise rate of 12 ℃/min, naturally cooling, last gained sample is the positive electrode material Li of doping Co 1+xCo 0.01V 2.99O 8
Embodiment 6:
With 1.05 * 10 -2Mol LiOHH 2O, 2.98 * 10 -2Mol NH 4VO 3, 4.47 * 10 -2Mol C 2H 5O 2N and 6.0 * 10 -5Mol2CoCO 33Co (OH) 2XH 2O mixes in beaker, adds deionized water and is diluted to 350ml.Then said mixture is carried out magnetic agitation 0.5h under 75 ℃, behind the homogeneous system to be formed, be poured in the crucible, and be placed on reacting by heating on the 800W electrothermal oven, regulating voltage is 200V.After treating the water evaporate to dryness, obtain presoma.This presoma ground be placed in the chamber type electric resistance furnace, be warming up to 430 ℃ with the temperature rise rate of 10 ℃/min, roasting 22h, naturally cooling, gained sample are the positive electrode material Li of doping Co 1+xCo 0.03V 2.97O 8
Embodiment 7:
With 1.05 * 10 -2Mol LiOHH 2O, 2.98 * 10 -2Mol NH 4VO 3, 4.47 * 10 -2Mol C 2H 5O 2N and 10.0 * 10 -5Mol 2CoCO 33Co (OH) 2XH 2O mixes in beaker, is diluted to 400ml with deionized water.Under 85 ℃ this mixture is stirred 0.6h under magnetic force, making it to form homogeneous system.Then this mixture is poured in the crucible, be placed on reacting by heating on the 800W electrothermal oven, control voltage is 200V.Behind the xerogel presoma to be formed, its grinding is placed in the chamber type electric resistance furnace, is warming up to 440 ℃, and at this roasting temperature 18h, the positive electrode material Li of the Co that promptly obtains behind the naturally cooling mixing with the temperature rise rate of 8 ℃/min 1+xCo 0.05V 2.95O 8
(3) Li 1+xCo yNi yV 3-2yO 8Preparation
In above example 1～4, get 2CoCO 33Co (OH) 2XH 2O, NiCO 32Ni (OH) 24H 2The LiOHH of O and metering 2O, NH 4VO 3And C 2H 5NO 2Mix in beaker together, add deionized water and be diluted to 300～400ml, in 70～85 ℃ of magnetic agitation 0.4-0.8h, make it to form homogeneous system, later operation is identical.
Embodiment 8:
With 1.05 * 10 -2Mol LiOHH 2O, 2.98 * 10 -2Mol NH 4VO 3, 4.47 * 10 -2Mol C 2H 5O 2N, 3.33 * 10 -5MolNiCO 32Ni (OH) 24H 2O and 2 * 10 -5Mol 2CoCO 33Co (OH) 2XH 2O mixes in beaker, is diluted to 300ml with deionized water.This mixture is carried out magnetic agitation 0.4h under 80 ℃, make it to form homogeneous system.Be poured in the crucible then, be placed on reacting by heating on the 800W electrothermal oven, by regulating voltage is 200V, after forming the xerogel presoma, this presoma ground be placed in the chamber type electric resistance furnace, be warming up to 420 ℃, constant temperature calcining 20h with the temperature rise rate of 12 ℃/min, naturally cooling, last gained sample is the positive electrode material Li of binary doped Co, Ni 1+xCo 0.01Ni 0.01V 2.98O 8
Embodiment 9:
With 1.05 * 10 -2Mol LiOHH 2O, 2.98 * 10 -2Mol NH 4VO 3, 4.47 * 10 -2Mol C 2H 5O 2N and 5.0 * 10 -5Mol NiCO 32Ni (OH) 24H 2O and 3.0 * 10 -5Mol 2CoCO 33Co (OH) 2XH 2O mixes in beaker, is diluted to 400ml with deionized water.Under 85 ℃ this mixture is stirred 0.6h under magnetic force, making it to form homogeneous system.Then this mixture is poured in the crucible, be placed on reacting by heating on the 800W electrothermal oven, control voltage is 200V.Behind the xerogel presoma to be formed, its grinding is placed in the chamber type electric resistance furnace, is warming up to 440 ℃ with the temperature rise rate of 8 ℃/min, and, promptly obtains the positive electrode material Li of binary doped Co, Ni behind the naturally cooling at this roasting temperature 20h 1+xCo 0.015Ni 0.015V 2.97O 8
Embodiment 10:
With 1.05 * 10 -2Mol LiOHH 2O, 2.98 * 10 -2Mol NH 4VO 3, 4.47 * 10 -2Mol C 2H 5O 2N and 6.66 * 10 -5Mol NiCO 32Ni (OH) 24H 2O and 4 * 10 -5Mol 2CoCO 33Co (OH) 2XH 2O mixes in beaker, adds deionized water and is diluted to 350ml.Then said mixture is carried out magnetic agitation 0.5h under 75 ℃, behind the homogeneous system to be formed, be poured in the crucible, and be placed on reacting by heating on the 800W electrothermal oven, regulating voltage is 210V.After treating the water evaporate to dryness, obtain presoma.This presoma ground be placed in the chamber type electric resistance furnace, be warming up to 430 ℃ with the temperature rise rate of 10 ℃/min, roasting 22h, naturally cooling, gained sample are the positive electrode material Li of binary doped Co, Ni 1+xCo 0.02Ni 0.02V 2.96O 8
Embodiment 11:
With 1.05 * 10 -2Mol LiOHH 2O, 2.98 * 10 -2Mol NH 4VO 3, 4.47 * 10 -2Mol C 2H 5O 2N and 10.0 * 10 -5Mol NiCO 32Ni (OH) 24H 2O and 6.0 * 10 -5Mol 2CoCO 33Co (OH) 2XH 2O mixes in beaker, is diluted to 400ml with deionized water.Under 85 ℃ this mixture is stirred 0.6h under magnetic force, making it to form homogeneous system.Then this mixture is poured in the crucible, be placed on reacting by heating on the 800W electrothermal oven, control voltage is 190V.Behind the xerogel presoma to be formed, its grinding is placed in the chamber type electric resistance furnace, is warming up to 440 ℃ with the temperature rise rate of 8 ℃/min, and, promptly obtains the positive electrode material Li of binary doped Co, Ni behind the naturally cooling at this roasting temperature 21h 1+xCo 0.03Ni 0.03V 2.94O 8
Embodiment 12:
With 1.05 * 10 -2Mol LiOHH 2O, 2.98 * 10 -2Mol NH 4VO 3, 4.47 * 10 -2Mol C 2H 5O 2N and 13.33 * 10 -5Mol NiCO 32Ni (OH) 24H 2O and 8.0 * 10 -5Mol 2CoCO 33Co (OH) 2XH 2O mixes in beaker, is diluted to 400ml with deionized water.Under 78 ℃ this mixture is stirred 0.6h under magnetic force, making it to form homogeneous system.Then this mixture is poured in the crucible, be placed on reacting by heating on the 800W electrothermal oven, control voltage is 180V.Behind the xerogel presoma to be formed, its grinding is placed in the chamber type electric resistance furnace, is warming up to 440 ℃ with the temperature rise rate of 8 ℃/min, and, promptly obtains the positive electrode material Li of binary doped Co, Ni behind the naturally cooling at this roasting temperature 19h 1+xCo 0.04Ni 0.04V 2.92O 8
Embodiment 13:
With 1.05 * 10 -2Mol LiOHH 2O, 2.98 * 10 -2Mol NH 4VO 3, 4.47 * 10 -2Mol C 2H 5O 2N and 16.66 * 10 -5Mol NiCO 32Ni (OH) 24H 2O and 10.0 * 10 -5Mol 2CoCO 33Co (OH) 2XH 2O mixes in beaker, is diluted to 400ml with deionized water.Under 82 ℃ this mixture is stirred 0.6h under magnetic force, making it to form homogeneous system.Then this mixture is poured in the crucible, be placed on reacting by heating on the 800W electrothermal oven, control voltage is 190V.Behind the xerogel presoma to be formed, its grinding is placed in the chamber type electric resistance furnace, is warming up to 440 ℃ with the temperature rise rate of 8 ℃/min, and, promptly obtains the positive electrode material Li of binary doped Co, Ni behind the naturally cooling at this roasting temperature 20h 1+xCo 0.05Ni 0.05V 2.90O 8

Claims (4)

1, a kind of anode material for lithium-ion batteries Li 1+xV 3O 8The preparation method, with lithium hydroxide and ammonium meta-vanadate is raw material, comprise mixing, reaction, evaporate to dryness, roasting and cooling, it is characterized in that: described mixing is a lithium hydroxide, ammonium meta-vanadate and glycine are dissolved in the deionized water after mixing, under 70～85 ℃ of conditions, be stirred to dissolving fully, reacting by heating and evaporate to dryness obtain presoma on electric furnace then, at last presoma is ground the back and be warming up to 420～450 ℃ with 8～15 ℃/min speed, and constant temperature calcining 18～22 hours, lithium during mixing/vanadium mol ratio is 0.90～1.15/3, and vanadium/glycine mol ratio is 1.0/1.2～1.8.
2, preparation method according to claim 1 is characterized in that: lithium during mixing/vanadium mol ratio is 1.05/3, and vanadium/glycine mol ratio is 1.0/1.5.
3, a kind of anode material for lithium-ion batteries Li 1+xCo yV 3-yO 8The preparation method, be at Li 1+xV 3O 8Mix in the preparation process, with lithium hydroxide, ammonium meta-vanadate is raw material, glycine is a complexing agent, comprise mixing, reaction, evaporate to dryness, roasting and cooling, it is characterized in that: getting cobaltous carbonate, to be mixed in the deionized water under 70～85 ℃ of conditions dispersed with stirring with lithium hydroxide, ammonium meta-vanadate and glycine even, and the add-on of cobaltous carbonate is: the Li/Co mol ratio is 1.0/0.01～0.05.
4, a kind of anode material for lithium-ion batteries Li 1+xCo yNi yV 3-2yO 8The preparation method, be at Li 1+xV 3O 8Mix in the preparation process, with lithium hydroxide, ammonium meta-vanadate is raw material, glycine is a complexing agent, comprise mixing, reaction, evaporate to dryness, roasting and cooling, it is characterized in that: getting cobaltous carbonate, nickelous carbonate, to be mixed in the deionized water under 70～85 ℃ of conditions dispersed with stirring with lithium hydroxide, ammonium meta-vanadate and glycine even, the add-on of cobaltous carbonate and nickelous carbonate is respectively: the Li/Co mol ratio is that 1.0/0.01～0.05, Li/Ni mol ratio are 1.0/0.01～0.05, and Co and Ni mol ratio are 1.0/1.0.
CNB2007100197486A 2007-02-09 2007-02-09 Preparation of positive electrode material Li(1+x)V3O8 of lithium ion cell and doping method Expired - Fee Related CN100480189C (en)

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CN114275812A (en) * 2021-12-23 2022-04-05 西安交通大学 graphene/LixV2O5Composite electrode material, preparation method and application thereof
CN114275812B (en) * 2021-12-23 2022-08-16 西安交通大学 graphene/Li x V 2 O 5 Composite electrode material, preparation method and application thereof
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