CN101504979A - A novel preparation method for LiFePO4/C composite positive pole material - Google Patents
A novel preparation method for LiFePO4/C composite positive pole material Download PDFInfo
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- CN101504979A CN101504979A CNA2009100569562A CN200910056956A CN101504979A CN 101504979 A CN101504979 A CN 101504979A CN A2009100569562 A CNA2009100569562 A CN A2009100569562A CN 200910056956 A CN200910056956 A CN 200910056956A CN 101504979 A CN101504979 A CN 101504979A
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Abstract
The invention discloses a LiFePO4/C composite anode material and a method for preparing the same, and in particular relates to a method for preparing a lithium ion buttery anode material. The LiFePO4/C composite anode material is synthesized by a liquid phase evaporation drying method, and the method comprises the following steps: firstly, according to a stoichiometric ratio, weighing certain amount of lithium source compounds, iron source compounds and phosphonium source compounds to prepare mixed solution with certain concentration, and adding right amount of carbon sources; secondly, synthesizing a precursor by controlling the reaction temperature, the stirring speed and the ultrasonic dispersion; thirdly, drying and grinding the precursor; and finally, processing the precursor powder at a temperature of between 500 and 800 DEG C for 2 to 15 hours, and cooling the product to room temperature to obtain the LiFePO4/C composite anode material. The method has the advantages of easy control, low energy consumption, short cycle, lithium source saving, low cost and the like; and the LiFePO4/C composite anode material prepared by the method has the characteristics of high purity, small particle size, even distribution of particles, good electrochemical performance and the like.
Description
Technical field
The invention belongs to the energy and material preparing technical field, specially refer to lithium ion battery LiFePO
4/ C composite positive pole and preparation method thereof.
Background technology
Positive electrode is the important component part of lithium ion battery, and has α-NaFeO
2The material of type structure is the research focus of positive electrode always.These materials comprise LiCoO
2, LiNiO
2, LiMn
2O
4Deng.LiCoO
2Be the positive electrode of present large-scale commercial, research comparative maturity, high comprehensive performance.But this material has tangible weak point, for example, costs an arm and a leg, and capacity is lower, and toxicity is bigger, has certain safety problem, and in addition, cobalt is a strategic resource, and reserves are limited.LiNiO
2Cost is lower, and capacity is higher, but its preparation difficulty and material property are extremely unstable, also have serious safety problem.In recent years, safety issue and the cost problem of people in order to solve lithium ion battery is to having the LiMn of spinel structure
2O
4Carry out a large amount of research, can solve LiCoO at present
2Cost problem and LiNiO
2Safety problem, but its cycle performance especially high temperature cyclic performance is poor, certain dissolubility is arranged in electrolyte, storge quality is poor.Therefore, need badly and develop novel positive electrode and satisfy the growing market demand.
LiFePO4 (the LiFePO of quadrature olivine structural
4) positive electrode becomes new research focus both at home and abroad gradually, and develop into anode material for lithium-ion batteries of new generation.This material does not contain noble element, raw material cheapness, aboundresources; Have higher specific capacity (theoretical specific capacity 170mAh/g), higher operating voltage (3.4V), good cycle performance, high-temperature behavior and security performance; Bulk effect is good when cooperating with carbon negative pole material, and is good with most of electrolyte compatibility; In addition, LiFePO
4Material is environmentally friendly, therefore more and more is subject to people's attention, and is considered to have the power lithium-ion battery positive electrode of application potential.
LiFePO
4Positive electrode is owing to FeO in the olivine structural
6The angle can't form the sort of continuous FeO that resembles in the structure of common limit altogether
6Therefore network configuration has influenced between the network of lithium ion and has flowed; Lithium ion can form FePO rapidly after taking off embedding simultaneously
4Phase can't form conducting electricity favourable transition state, makes LiFePO
4Ionic conduction and electron conductivity all lower, Li when discharging and recharging
+At LiFePO
4-FePO
4Diffusion coefficient between the two-phase is less, causes LiFePO
4Actual specific capacity and high rate during charging-discharging are relatively poor.At present, the major measure of raising LiFePO4 conductivity has:
(1) adds conductive agent, mainly, improve conductivity of electrolyte materials by realizing at LiFePO4 particle surface coated with conductive material with carbon element or conducting metal.
(2) element doping mixes high price foreign metal ion, as Mg in the LiFePO4 lattice
2+, Al
3+, Cr
3+, Ti
4+Deng, replace a part of Li
+Or Fe
2+The position, thereby make the LiFePO4 intrinsic semiconductor change n type or p N-type semiconductor N into, this method is the highest can to improve conductivity of electrolyte materials 8 orders of magnitude.
(3) reduce particle diameter, the synthetic less LiFePO4 particle of particle diameter shortens lithium ion the evolving path in material, increases the contact area of material and electrolyte, thereby improves the diffusion rate of lithium ion in material.
Method preparing phosphate iron lithium mainly contains solid phase method, liquid-phase precipitation method etc.
Traditional solid phase method is as (Improved electrochemical performanceof a LiFePO such as P.P.Prosini
4-based composite cathode[J] .Electrochem Acta; 46 (2001): 3517-3523) with molysite such as ferrous oxalate or ferric nitrate, ammonium dihydrogen phosphate and lithium salts such as lithium carbonate or lithium hydroxide by metering than mixing; under inert gas shielding, roasting becomes LiFePO4.The advantage of this method is that technology is simple, is easy to realize industrialization, but the common mixing of reactant is inhomogeneous, and the product particle is bigger, and purity is not high, chemical property is undesirable, and this method energy consumption is big, and energy utilization rate is low.
Liquid-phase precipitation method is with after the suitable raw material dissolving, adds other compounds to separate out precipitation, obtains product after drying, the roasting.As (Size Effects on Carbon-FreeLiFePO such as C.Delacout
4Powers, The Key to Superior Energy Density[J] .Electrochemical andSolid-State Letters, 2006,9 (7): A352-A355) adopt liquid-phase precipitation method, regulate the pH value and the ferric lithium phosphate precursor particle is precipitated out in the aqueous solution, obtain LiFePO4 after drying, the roasting near neutral (5.6～8.2).The advantage of liquid-phase precipitation method is that precursor reagent is dispersed in and can reaches molecular level in the liquid phase and mix, and the product particle diameter that calcining obtains is little, chemical property is good, and forerunner's physical efficiency of this method realizes that low temperature is synthetic.But this procedure control is strict, and technology is loaded down with trivial details, waste lithium source (the lithium consumption is 3 times of theoretical consumption), and it is synthetic only to be adapted at the laboratory basically.
The invention discloses the synthetic LiFePO of a kind of liquid phase steam seasoning
4The technology of/C composite positive pole.
Summary of the invention
The present invention aims to provide that a kind of technology is simple, with low cost, raw material saving, productive rate height, be fit to the method preparing phosphate iron lithium of suitability for industrialized production.At LiFePO
4There are problems such as the low and high rate during charging-discharging of actual specific capacity is relatively poor in material, and the shortcoming of solid phase method and liquid-phase precipitation method, has developed a kind of method of liquid phase evaporate to dryness synthesizing iron lithium phosphate.Adopt the synthetic lithium iron phosphate positive material of this method to have height ratio capacity, high-energy-density and excellent cycle stability, can adapt to the lithium ion power battery cathode material of high current charge-discharge.
Adopt liquid phase steam seasoning synthesizing iron lithium phosphate positive electrode, its know-why comprises:
(1) presoma is synthetic, by control solution concentration, reaction temperature, the ultrasonic synthetic presoma of stir speed (S.S.) and interval.
(2) drying of presoma, adopt microwave drying and (or) infrared radiation drying.
Described LiFePO
4/ C composite positive pole and liquid phase evaporate to dryness synthetic method thereof comprise the steps:
(1) presoma is synthetic: take by weighing a certain amount of Fe source compound, Li source compound, P source compound, and water-solublely be made into certain density mixed solution, add proper amount of carbon source again in mixed solution, mix.Then reaction vessel is placed 60～100 ℃ of water-baths, stir speed (S.S.) is 50～250r/min, and carries out suitable ultrasonic dispersion, at last up to the mixed solution evaporate to dryness is obtained precursor.Wherein, the mol ratio of Fe source compound, Li source compound, P source compound consumption is: the preferred Fe:Li:P=1.0:1.0:1.0 in Fe:Li:P=1.0～1.1:1.0～1.1:1.0～1.1; When carrying out ultrasonic dispersion, each ultrasonic time is 5～15 minutes, ultrasonicly is spaced apart 10～30 minutes, and ultrasonic number of times is 1～3 time.
(2) drying of presoma: will place infrared drying oven to carry out drying through the presoma that step (1) obtains, the power of drying box be 250～1000W, and irradiation time is 2～12 hours; (or) place microwave oven to carry out drying, microwave power is 100～600W, be 3～30 minutes heating time.After drying finishes presoma is taken out grind into powder.
(3) sintering: put into high temperature furnace through the precursor powder that step (2) obtains, in the mixed atmosphere of hydrogen and argon gas, be raised to 500～800 ℃ from room temperature, be incubated 2～15 hours again, promptly obtain LiFePO after naturally cooling to room temperature with the heating rate of 2～10 ℃/min
4/ C composite positive pole.Wherein argon gas and hydrogen volume flow-rate ratio are 5～11.
Described Fe source compound is a ferric nitrate; Li source compound is selected from a kind of or its mixture in lithium dihydrogen phosphate, lithium hydroxide, lithium acetate, the lithium nitrate; P source compound is selected from a kind of or its mixture in lithium dihydrogen phosphate, phosphoric acid hydrogen two lithiums, phosphoric acid, diammonium hydrogen phosphate, the ammonium dihydrogen phosphate; Carbon source is selected from a kind of or its mixture in polyethylene glycol (PEG), polyvinyl alcohol (PVA), softex kw (CTAB), the sucrose, and the carbon source consumption is LiFePO
44～25% of Theoretical Mass.
The lithium iron phosphate positive material that utilizes the present invention to prepare, granularity be less than 700nm, even particle distribution, first discharge specific capacity 〉=150mAh/g under the 0.1C, good cycling stability.
Advantage of the present invention:
(1) can regulate and control the size of synthetic LiFePO4 particle by controlling solution concentration, reaction temperature, stir speed (S.S.) and ultrasonic time;
(2) adopting cheap ferric iron is source of iron, has avoided the waste in lithium source simultaneously;
(3) He Cheng material particle size is little, specific capacity is high, good cycle, good heavy current;
(4) preparation technology is simple, the cycle is short, with low cost, suitable large-scale production.
Description of drawings
The LiFePO of Fig. 1 for making by embodiment 1 technology
4The XRD figure of/C positive electrode.
The LiFePO of Fig. 2 for making by embodiment 2 technologies
4The SEM figure of/C composite positive pole.
The LiFePO of Fig. 3 for making by embodiment 3 technologies
4The first charge-discharge curve chart of/C composite positive pole under 0.1C, voltage range is 2.5～4.2V, electrolyte is the LiPF of 1.0mol/L
6(EC/DMC=1:1, volume ratio).
The LiFePO of Fig. 4 for making by embodiment 3 technologies
4/ C composite positive pole is cycle performance figure under 0.1C.
The LiFePO of Fig. 5 for making by embodiment 4 technologies
4/ C composite positive pole is cycle performance figure under 0.1C-0.5C-1C.
Embodiment
Below by EXPERIMENTAL EXAMPLE the present invention is specifically described; it is important to point out that present embodiment only is used for that the present invention will be further described; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1
Take by weighing a certain amount of lithium acetate, ferric nitrate, diammonium hydrogen phosphate according to stoichiometric proportion, be dissolved in deionized water and be made into the mixed solution that concentration is 2mol/L, take by weighing LiFePO then
4The PVA of Theoretical Mass 10% stirs in the mixed liquor of adding front.Then reaction vessel is placed water-bath, setting bath temperature is 80 ℃, and stir speed (S.S.) is 100r/min, when muddy state appears in solution, begin ultrasonic dispersion, each ultrasonic jitter time is 5 minutes, ultrasonic interval 10 minutes, ultrasonic 3 times altogether, obtain presoma up to the solution evaporate to dryness at last, taking out presoma and placing infrared drying oven and regulate power is 250W, dry 10 hours,, obtain the dry precursor solid, the solid abrasive powdered is carried out sintering.Heat treatment process is raised to 600 ℃ from room temperature with the heating rate of 5 ℃/min, 600 ℃ down insulation naturally cool to room temperature and promptly obtain LiFePO after 5 hours
4/ C composite positive pole.The product of gained is indicated as single olivine-type LiFePO through X-ray diffraction analysis
4Structure (as Fig. 1).
Embodiment 2
Take by weighing a certain amount of lithium hydroxide, ferric nitrate, ammonium dihydrogen phosphate according to stoichiometric proportion, be dissolved in deionized water and be made into the solution that concentration is 1.5mol/L, take by weighing LiFePO then
4The CTAB of Theoretical Mass 5% stirs in the mixed liquor of adding front.Then reaction vessel is placed water-bath, setting bath temperature is 70 ℃, and stir speed (S.S.) is 200r/min, when muddy state appears in solution, begin ultrasonic dispersion, each ultrasonic jitter time is 6 minutes, ultrasonic interval 15 minutes, ultrasonic 2 times altogether, obtain presoma up to the solution evaporate to dryness at last, take out presoma and place microwave oven, controlled microwave power is 300W heating 15 minutes, obtain the dry precursor solid, grind into powder carries out sintering then.Heat treatment process is raised to 600 ℃ from room temperature with the heating rate of 10 ℃/min, 600 ℃ down insulation naturally cool to room temperature after 3 hours and promptly obtain LiFePO
4/ C composite positive pole, SEM (Fig. 2) shows this product even particle distribution, particle size distribution is in 200～300nm scope.
Take by weighing a certain amount of lithium dihydrogen phosphate, ferric nitrate according to stoichiometric proportion, be dissolved in deionized water and be made into the solution that concentration is 1mol/L, take by weighing LiFePO then
4PEG of Theoretical Mass 10% (mean molecule quantity is 380～400) and 5% sucrose add these two kinds of mixed carbon sources in the mixed liquor of fronts and stir.Then reaction vessel is placed water-bath, setting bath temperature is 90 ℃, stir speed (S.S.) is 150r/min, when muddy state appearred in solution, ultrasonic dispersion 15 minutes obtained presoma up to the solution evaporate to dryness at last, taking out presoma and placing infrared drying oven and regulate power is 500W, dry 6 hours, obtain the dry precursor solid, then grind into powder.Heat treatment process is raised to 700 ℃ from room temperature with the heating rate of 10 ℃/min, 700 ℃ down insulation naturally cool to room temperature after 3 hours and promptly obtain LiFePO
4/ C composite positive pole.The product of gained is assembled into Experimental cell, and usefulness constant current charge-discharge technology is measured its charging and discharging capacity and cycle performance, the first discharge specific capacity of 0.1C such as Fig. 3, cycle performance such as Fig. 4 that the following circulation of 0.1C is 40 times.
Embodiment 4
Take by weighing a certain amount of lithium acetate, ferric nitrate, diammonium hydrogen phosphate according to stoichiometric proportion, be dissolved in deionized water and be made into the mixed solution that concentration is 1.5mol/L, take by weighing LiFePO then
4The PEG of Theoretical Mass 20% (mean molecule quantity is 380～400) stirs in the mixed liquor of adding front.Then reaction vessel is placed water-bath, setting bath temperature is 100 ℃, and stir speed (S.S.) is 50r/min, when muddy state appears in solution, begin ultrasonic dispersion, each ultrasonic jitter time is 7 minutes, ultrasonicly is spaced apart 10 minutes, ultrasonic 2 times altogether, obtain presoma up to the solution evaporate to dryness at last, take out presoma and place microwave oven, controlled microwave power is 500W heating 6 minutes, obtain the dry precursor solid, solid is taken out grind into powder.Heat treatment process is raised to 700 ℃ from room temperature with the heating rate of 7 ℃/min, 700 ℃ down insulation naturally cool to room temperature after 3 hours and promptly obtain LiFePO
4/ C composite positive pole is assembled into Experimental cell with the product of gained, carries out the charge-discharge performance test under 0.1C-0.5C-1C, the results are shown in Figure 5.
Claims (10)
1, the synthetic LiFePO of liquid phase steam seasoning
4/ C composite positive pole is characterized in that comprising the steps:
(1) presoma is synthetic: take by weighing a certain amount of Fe source compound, Li source compound, P source compound, and water-solublely be made into certain density mixed solution, add an amount of carbon source again in mixed solution, mix.Then reaction vessel is placed water-bath, by control bath temperature, stir speed (S.S.) and suitable ultrasonic dispersion, at last up to the mixed solution evaporate to dryness is obtained presoma.Wherein the mol ratio of Fe source compound, Li source compound, P source compound consumption is: Fe:Li:P=1.0～1.1:1.0～1.1:1.0～1.1, preferred Fe:Li:P=1.0:1.0:1.0.
(2) drying of presoma: will place through the presoma that step (1) obtains infrared drying oven carry out infrared radiation dry and (or) place microwave oven to carry out microwave drying.After drying finishes presoma is taken out grind into powder.
(3) sintering: put into high temperature furnace through the precursor powder that step (2) obtains, in the mixed atmosphere of hydrogen and argon gas, be raised to 500～800 ℃ from room temperature, be incubated 2～15 hours again, promptly obtain LiFePO after naturally cooling to room temperature with the heating rate of 2～10 ℃/min
4/ C composite positive pole.Wherein argon gas and hydrogen volume flow-rate ratio are 5～11.
2, the synthetic LiFePO of liquid phase steam seasoning according to claim 1
4/ C composite positive pole is characterized in that the mixed solution of the Fe source compound described in the step (1), Li source compound, P source compound, and its concentration range is 0.5～3mol/L.
3, the synthetic LiFePO of liquid phase steam seasoning according to claim 1
4/ C composite positive pole is characterized in that it is 5～15 minutes that ultrasonic described in the step (1) is separated into each ultrasonic time, ultrasonicly is spaced apart 10～30 minutes, and ultrasonic number of times is 1～3 time.
4, the synthetic LiFePO of liquid phase steam seasoning according to claim 1
4/ C composite positive pole is characterized in that the bath temperature described in the step (1) is 60～100 ℃.
5, the synthetic LiFePO of liquid phase steam seasoning according to claim 1
4/ C composite positive pole is characterized in that the stir speed (S.S.) described in the step (1) is 50～250r/min.
6, the synthetic LiFePO of liquid phase steam seasoning according to claim 1
4/ C composite positive pole, the power that it is characterized in that the infrared drying oven described in the step (2) is 250～1000W, shines 2～12 hours; Microwave power is 100～600W, heats 3～30 minutes.
7, the synthetic LiFePO of liquid phase steam seasoning according to claim 1
4/ C composite positive pole is characterized in that the Fe source compound described in the step (1) is a ferric nitrate.
8, the synthetic LiFePO of liquid phase steam seasoning according to claim 1
4/ C composite positive pole is characterized in that the Li source compound described in the step (1) is selected from a kind of or its mixture in lithium dihydrogen phosphate, lithium hydroxide, lithium acetate, the lithium nitrate.
9, the synthetic LiFePO of liquid phase steam seasoning according to claim 1
4/ C composite positive pole is characterized in that the P source compound described in the step (1) is selected from a kind of or its mixture in lithium dihydrogen phosphate, phosphoric acid hydrogen two lithiums, phosphoric acid, diammonium hydrogen phosphate, the ammonium dihydrogen phosphate.
10, the synthetic LiFePO of liquid phase steam seasoning according to claim 1
4/ C composite positive pole is characterized in that the carbon source described in the step (1) is selected from a kind of or its mixture in polyethylene glycol (PEG), polyvinyl alcohol (PVA), softex kw (CTAB), the sucrose; The carbon source consumption is LiFePO
44～25% of Theoretical Mass.
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