CN104485450B - A kind of lithium ion battery negative material FeV2o4preparation method - Google Patents
A kind of lithium ion battery negative material FeV2o4preparation method Download PDFInfo
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
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Abstract
A kind of lithium ion battery negative material FeV2O4Preparation method; comprise the following steps: (1) by Ferrox. solution and ammonium metavanadate solution in ferrous ion and vanadium ion concentration than the ratio for 1:2; under protective atmosphere; it is added simultaneously in stirred autoclave be stirred; reaction; regulation pH to 2～6, continues reaction 1～4h, obtains navy blue suspension；(2) addition of step (1) gained suspension is equivalent to its volume 1～the ethanol of 3%, is then spray-dried, obtains presoma material；(3) by step (2) gained presoma material under protective atmosphere, in 200～400 DEG C of heat treatments 8～15h, add liquid nitrogen quenching, obtain lithium ion battery negative material FeV2O4.The inventive method heat treatment reaction temperature is low, obtained FeV2O4Negative material granule has microspheroidal structure, and tap density is high, and has higher charge-discharge characteristic and good cycle life.
Description
Technical field
The present invention relates to the preparation method of a kind of lithium ion battery negative material, be specifically related to a kind of lithium ion battery negative material FeV2O4Preparation method.
Background technology
At present, in the commercially producing of battery, battery cathode mainly uses graphite manufacture, but either native graphite or Delanium, its theoretical specific capacity is all only 372mAh/g.The advantage that although graphite cathode has inexpensively, safety is good, but along with the exploitation of some height ratio capacity positive electrodes, the graphite of relatively low specific capacity can not meet the requirement matched with positive electrode as negative pole.
Novel negative material emerges in an endless stream, such as lithium titanate, agraphitic carbon, Si-C composite material, kamash alloy, metal alloy, Graphene etc..Although Novel anode material differs from one another, but there is presently no any material and have absolute advantages, various new materials are also actively being researched and developed by each enterprise, mechanism.Such as lithium titanate good cycle, but theoretical capacity only has 175mAh/g, and volume and capacity ratio does not has advantage especially, it is difficult to meet the requirement to cell high-capacity of electric motor car and hybrid electric vehicle.Therefore, exploitation have height ratio capacity, high charge-discharge efficiencies, long circulation life Novel cathode material for lithium ion battery pole the most urgent.
The biggest difference is there is because the kind of material is different in the specific discharge capacity of electrode, cycle performance with the stationarity of charge and discharge curve.Such as Li3FeN2During as cathode of lithium battery, discharge capacity is 150mAh/g, discharge potential is at 1.3V(vs Li/Li+Near), charge and discharge curve is the most smooth, and discharge off is delayed, but capacity has substantially decay；Li3-xCoxN has the high discharge capacity of 900mAh/g, and discharge potential is at about 1.0V, but charge and discharge curve is less steady, has obvious current potential delayed and capacity attenuation.At present, this kind of material to reach actual application, in addition it is also necessary to furthers investigate further.When the metals such as some metal such as Sn, Si, Al embed lithium, it will form lithium-metal alloy that the amount Han lithium is the highest, if the theoretical capacity of Sn is 990mAh/cm3, close to 10 times of the theoretical volume specific capacity of graphite.But the subject matter of alloy material of cathode is the most inefficient and cyclical stability is poor, it is necessary to solve the problem that negative material bulk effect during repeated charge causes electrode structure to destroy.And simple metal material negative pole cycle performance is very poor, safety is the most bad.F.F.Tao etc. use wet chemical method to synthesize the Co of diameter 3～7 μm that nanometer sheet is self-assembly of3O4Tiny balloon, nanometer sheet is made up of the nano-particle of diameter about 50nm, and first discharge specific capacity is 1048mAh/g, but just decays to 390mAh/g to second circulation specific discharge capacity.The method of solvent thermal and calcining such as L.Liu has synthesized nanometer chip base NiO microsphere, find that temperature, time and the surfactant of reaction have material impact for product morphology, during 50mA/g constant current charge-discharge, first discharge specific capacity about 1570mAh/g, but during charging, special capacity fade reaches 500mAh/g, and cyclical stability is poor.
At present, China's vanadium, iron resource are abundant, and raw material sources is extensive, with low cost.Therefore, FeV2O4It it is a lithium ion battery negative material with the biggest potentiality and value.Laboratory can prepare FeV by solid-phase ball milling method at present2O4, but various aspects of performance is the most poor.
Summary of the invention
The technical problem to be solved is to provide that a kind of synthesis temperature is low, and condition is easily controllable, and synthetic method is simple, product tap density and electrochemical performance, utilizes the lithium ion battery negative material FeV being spray-dried collaborative heat treatment quenching technology2O4Preparation method.
The technical solution adopted for the present invention to solve the technical problems is: a kind of lithium ion battery negative material FeV2O4Preparation method, comprise the following steps:
(1) by Ferrox. solution and ammonium metavanadate solution in solution ferrous ions and the ratio of vanadium ion mol ratio 1:2; under protective atmosphere; it is added simultaneously in stirred autoclave stirring reaction; after charging terminates; regulation pH value of solution is to 2～6(preferably 4～5.5); continue reaction 1～4h(preferably 1.5～3h), obtain navy blue suspension；
(2) addition of step (1) gained suspension is equivalent to its volume 1～the ethanol of 3%, is then spray-dried, obtains presoma material；
(3) by step (2) gained presoma material under protective atmosphere, in 200～400 DEG C of (preferably 300～380 DEG C) heat treatments 8～15h(preferably 9～12h), add liquid nitrogen quenching, obtain lithium ion battery negative material FeV2O4。
Further, in step (1), described Ferrox. solution and ammonium metavanadate solution are 200～600mL/h(preferably 300～500mL/h by the speed that solution adds).
Further, in step (2), the charging rate of described spray drying is 400～1200 mL/h(preferably 600～1000 mL/h), dry inlet temperature is 150～250 DEG C (preferably 200～230 DEG C), and leaving air temp is 80～150 DEG C (preferably 100～130 DEG C).
Further, in step (1), the speed of described stirring is 200～400rpm(preferably 250～350rpm).
Further, in step (1) and (3), described protective atmosphere is one or more in argon, nitrogen, hydrogen, carbon dioxide or carbon monoxide.
In step (2), the ethanol of described addition can play the effect of discrete particles, and is spray-dried the effect that can play spheroidizing of particles.
In step (3), after by presoma material heat treatment, carry out quenching and material can be made finer and close.
The inventive method is to utilize to be spray-dried collaborative heat treatment quenching technology to prepare ion battery cathode material FeV2O4, granule dispersion in the suspension that synthetic reaction obtains can be made more uniform, the most uniform with the presoma composition that this obtains.Gained lithium ion battery negative material FeV of the present invention2O4Having microspheroidal structure (mean diameter about 3 μm), owing to micro-sphere structure can make material finer and close, it is possible to be effectively improved the Physical Processing performance of negative material, improve a lot the tap density of material especially, tap density is by 1.14g/cm3Bring up to 1.72g/cm3So that the volume energy density of battery increases by 50%.On the other hand, FeV2O4Similar with graphite, alloy and metal-oxide, the deintercalation site of lithium ion is equally provided, and owing to vanadium has active chemical property (V2+To V5+), therefore, FeV2O4There is higher specific capacity (～800mAh/g), gained lithium ion battery negative material FeV of the present invention2O4Under 0.1～2.5V voltage, 0.1C first discharge specific capacity still keeps 652.6mAh/g after circulating 50 times up to 866.5mAh/g, 1C first discharge specific capacity up to 708.2mAh/g, 0.1C.Therefore, gained lithium ion battery negative material FeV of the present invention2O4There is the chemical property of excellence, present good cycle life, the shortcoming effectively solving metal-oxide negative material capacity attenuation.The raw materials used wide material sources of the present invention, technological process is simple, reacts temperature required low, and granule has microspheroidal structure, and tap density is high, and has higher charge-discharge characteristic and good cycle life.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the embodiment of the present invention 1 sample；
Fig. 2 is the SEM diffraction pattern of the embodiment of the present invention 1 sample；
Fig. 3 is 0.1C, 1C discharge curve first of the embodiment of the present invention 1 sample；
Fig. 4 is the discharge cycles figure under the 0.1C multiplying power of the embodiment of the present invention 1 sample；
Fig. 5 is 0.1C, 1C discharge curve first of comparative example 1 sample of the present invention；
Fig. 6 is the discharge cycles figure under the 0.1C multiplying power of comparative example 1 sample of the present invention.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the invention will be further described.
Embodiment
1
(1) 0.01mol Ferrox. is dissolved in the deionized water of 100mL it is made into the solution that concentration is 0.1mol/L；0.02mol ammonium metavanadate is dissolved in the deionized water of 100mL and is made into the solution that concentration is 0.2mol/L；The Ferrox. solution prepared and ammonium metavanadate solution are all joined in stirred autoclave with the speed of 400mL/h under high pure nitrogen (concentration >=99.99%) atmosphere the most simultaneously, control mixing speed is 300rpm, charging regulates pH to 5 with ammonia after terminating, continue reaction 2h, obtain navy blue suspension；(2) by adding the ethanol of 4mL in step (1) gained suspension, being then spray-dried, charging rate is 800 mL/h, and dry inlet temperature is 220 DEG C, and leaving air temp is 120 DEG C, obtains presoma material；(3) by step (2) gained presoma material under the protection of high pure nitrogen (concentration >=99.99%) in 350 DEG C of heat treatment 10h, add 2mL liquid nitrogen and carry out quenching, obtain lithium ion battery negative material FeV2O4, tap density is 1.72g/cm3。
As shown in Figure 1, FeV2O4Crystalline structure tend to amorphous state, there is no complete crystal structure；As shown in Figure 2, FeV2O4Pattern be spherical, the consistency of product is high.
The assembling of battery: weigh the FeV obtained by 0.4g2O4, add 0.05g acetylene black and make conductive agent and 0.05g NMP(N-methyl pyrrolidone) and make binding agent, it is coated in after mix homogeneously on Copper Foil and makes negative plate, with metal lithium sheet as positive pole in vacuum glove box, with Celgard 2300 as barrier film, 1mol/L LiPF6/ EC:DMC(volume ratio 1:1) it is electrolyte, be assembled into the button cell of CR2025,0.1C first discharge specific capacity is that 866.5mAh/g(sees Fig. 3), after 50 circulations, specific discharge capacity still reaches 652.6mAh/g(and sees Fig. 4)；1C first discharge specific capacity is that 708.2 mAh/g(see Fig. 3).
Embodiment
2
(1) 0.01mol Ferrox. is dissolved in the deionized water of 100mL it is made into the solution that concentration is 0.1mol/L；0.02mol ammonium metavanadate is dissolved in the deionized water of 100mL and is made into the solution that concentration is 0.2mol/L；The Ferrox. solution prepared and ammonium metavanadate solution are all joined in stirred autoclave with the speed of 200mL/h under high-purity argon gas (concentration >=99.99%) atmosphere the most simultaneously, control mixing speed is 200rpm, charging regulates pH to 2 with ammonia after terminating, continue reaction 1h, obtain navy blue suspension；(2) by adding the ethanol of 2mL in step (1) gained suspension, being then spray-dried, charging rate is 400 mL/h, and dry inlet temperature is 150 DEG C, and leaving air temp is 80 DEG C, obtains presoma material；(3) by step (2) gained presoma material under the protection of high-purity argon gas (concentration >=99.99%) in 200 DEG C of heat treatment 8h, add 1mL liquid nitrogen and carry out quenching, obtain lithium ion battery negative material FeV2O4, tap density is 1.58g/cm3。
The assembling of battery: weigh the FeV obtained by 0.4g2O4, add 0.05g acetylene black and make conductive agent and 0.05g NMP(N-methyl pyrrolidone) and make binding agent, it is coated in after mix homogeneously on Copper Foil and makes negative plate, with metal lithium sheet as positive pole in vacuum glove box, with Celgard 2300 as barrier film, 1mol/L LiPF6/ EC:DMC(volume ratio 1:1) it is electrolyte, it is assembled into the button cell of CR2025,0.1C first discharge specific capacity is 786.5mAh/g, and after 50 circulations, specific discharge capacity is 601.8mAh/g；1C first discharge specific capacity is 650.2 mAh/g.
Embodiment
3
(1) 0.01mol Ferrox. is dissolved in the deionized water of 100mL it is made into the solution that concentration is 0.1mol/L；0.02mol ammonium metavanadate is dissolved in the deionized water of 100mL and is made into the solution that concentration is 0.2mol/L；The Ferrox. solution prepared and ammonium metavanadate solution are all joined in stirred autoclave with the speed of 600mL/h under high-purity argon gas (concentration >=99.99%) atmosphere the most simultaneously, control mixing speed is 400rpm, charging regulates pH to 6 with ammonia after terminating, continue reaction 4h, obtain navy blue suspension；(2) by adding the ethanol of 6mL in step (1) gained suspension, being then spray-dried, charging rate is 1200 mL/h, and dry inlet temperature is 250 DEG C, and leaving air temp is 150 DEG C, obtains presoma material；(3) by step (2) gained presoma material under the protection of high-purity argon gas (concentration >=99.99%) in 400 DEG C of heat treatment 15h, add 5mL liquid nitrogen and carry out quenching, obtain lithium ion battery negative material FeV2O4, tap density is 1.62g/cm3。
The assembling of battery: weigh the FeV obtained by 0.4g2O4, add 0.05g acetylene black and make conductive agent and 0.05g NMP(N-methyl pyrrolidone) and make binding agent, it is coated in after mix homogeneously on Copper Foil and makes negative plate, with metal lithium sheet as positive pole in vacuum glove box, with Celgard 2300 as barrier film, 1mol/L LiPF6/ EC:DMC(volume ratio 1:1) it is electrolyte, it is assembled into the button cell of CR2025,0.1C first discharge specific capacity is 796.5mAh/g, and after 50 circulations, specific discharge capacity is 611.7mAh/g；1C first discharge specific capacity is 685.2 mAh/g.
Comparative example
1
(1) 0.01mol Ferrox. and 0.02mol ammonium metavanadate directly being carried out under high pure nitrogen (concentration >=99.99%) atmosphere ball milling, control ball milling speed is 300r/min, and Ball-milling Time is 2h, obtains presoma material；(2) by step (1) gained presoma material under the protection of high pure nitrogen (concentration >=99.99%) in 350 DEG C of heat treatment 10h, add 2mL liquid nitrogen, obtain lithium ion battery negative material FeV2O4, tap density is 1.14g/cm3。
The assembling of battery: weigh the FeV obtained by 0.4g2O4, add 0.05g acetylene black and make conductive agent and 0.05g NMP(N-methyl pyrrolidone) and make binding agent, it is coated in after mix homogeneously on Copper Foil and makes negative plate, with metal lithium sheet as positive pole in vacuum glove box, with Celgard 2300 as barrier film, 1mol/L LiPF6/ EC:DMC(volume ratio 1:1) it is electrolyte, it is assembled into the button cell of CR2025,0.1C first discharge specific capacity is that 778.9mAh/g(sees Fig. 5), after 50 circulations, specific discharge capacity is that 226.4mAh/g(sees Fig. 6)；1C first discharge specific capacity is that 557.2 mAh/g(see Fig. 5).
Compared with example 1, the tap density of product is the most on the low side, and, chemical property is the most poor, and especially cyclical stability is poor.
Claims (9)
1. a lithium ion battery negative material FeV2O4Preparation method, it is characterised in that: comprise the following steps:
(1) by Ferrox. solution and ammonium metavanadate solution in solution ferrous ions and the ratio of vanadium ion mol ratio 1:2, under protective atmosphere, stirring reaction it is added simultaneously in stirred autoclave; after charging terminates; regulation pH value of solution, to 2～6, continues reaction 1～4h, obtains navy blue suspension；
(2) addition of step (1) gained suspension is equivalent to its volume 1～the ethanol of 3%, is then spray-dried, obtains presoma material；The charging rate of described spray drying is 400～1200
ML/h, dry inlet temperature is 150～250 DEG C, and leaving air temp is 80～150 DEG C；
(3) by step (2) gained presoma material under protective atmosphere, in 200～400 DEG C of heat treatments 8～15h, add liquid nitrogen quenching, obtain lithium ion battery negative material FeV2O4。
Lithium ion battery negative material FeV the most according to claim 12O4Preparation method, it is characterised in that: in step (1), described Ferrox. solution and ammonium metavanadate solution are 200～600mL/h by the speed that solution adds.
Lithium ion battery negative material FeV the most according to claim 1 or claim 22O4Preparation method, it is characterised in that: in step (1), the speed of described stirring is 200～400rpm.
Lithium ion battery negative material FeV the most according to claim 1 or claim 22O4Preparation method, it is characterised in that: in step (1) and (3), described protective atmosphere is one or more in argon, nitrogen, hydrogen, carbon dioxide or carbon monoxide.
Lithium ion battery negative material FeV the most according to claim 1 or claim 22O4Preparation method, it is characterised in that: in step (1), regulation pH value of solution to 4～5.5, continue reaction time be 1.5～3h.
Lithium ion battery negative material FeV the most according to claim 1 or claim 22O4Preparation method, it is characterised in that: in step (3), the temperature of described heat treatment is 300～380 DEG C, and the time is 9～12h.
Lithium ion battery negative material FeV the most according to claim 22O4Preparation method, it is characterised in that: in step (1), described Ferrox. solution and ammonium metavanadate solution are 300～500mL/h by the speed that solution adds.
Lithium ion battery negative material FeV the most according to claim 12O4Preparation method, it is characterised in that: in step (2), the charging rate of described spray drying is 600～1000
ML/h, dry inlet temperature is 200～230 DEG C, and leaving air temp is 100～130 DEG C.
Lithium ion battery negative material FeV the most according to claim 32O4Preparation method, it is characterised in that: in step (1), the speed of described stirring is 250～350rpm.
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