CN102263248B - Method for preparing carbon coated nanometer LiFePO4 - Google Patents
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- CN102263248B CN102263248B CN201110177626.6A CN201110177626A CN102263248B CN 102263248 B CN102263248 B CN 102263248B CN 201110177626 A CN201110177626 A CN 201110177626A CN 102263248 B CN102263248 B CN 102263248B
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Abstract
The invention discloses a method for preparing carbon coated nanometer LiFePO4 and belongs to the technical field of preparation of a positive pole material of a lithium ion battery. The method comprises the following steps: dissolving or dispersing nanometer iron phosphate, a nanometer lithium salt and a carbon source which are taken in a molar ratio of Fe to Li to C of 1:1: (1-5) to a solvent so as to obtain a stable and uniform nanometer fluid, and then rapidly removing the solvent in the nanometer fluid, thereby obtaining a uniformly mixed solid particle reactant; and roasting the uniformly mixed solid particle reactant in a hydrogen atmosphere, inert gas atmosphere or mixed gas atmosphere composed of hydrogen and inert gas, so as to obtain carbon coated nanometer LiFePO4. The preparation method disclosed by the invention is high in production efficiency and is easy to implement; and the size of the obtained carbon coated nanometer LiFePO4 particle is in a nanometer level and is narrow in distribution, and the carbon film of the particle is uniform, thereby being beneficial to improvements of ion transfer and conductivity and improvement of consistence of lithium ion battery positive pole materials.
Description
Technical field
The invention belongs to the anode material for lithium-ion batteries preparing technical field, particularly a kind of method for preparing the nano-lithium iron phosphate of carbon coating.Be specially a kind of method that solid phase method prepares the nano-lithium iron phosphate of even carbon coating.
Background technology
With conventional batteries, compare, lithium ion battery has a clear superiority on energy density, therefore rapidly at light movable equipment as notebook computer, digital camera, be widely applied on mobile phone etc.In lithium ion battery, the performances such as the capacitance of negative material, conductivity are far above positive electrode, so positive electrode has determined battery performance.But traditional positive electrode is as cobalt acid lithium, and LiMn2O4 etc. has such as poor heat stability, poor chemical stability, the shortcoming such as cycle performance is poor.And lithium ion battery has higher requirement as the application in the fields such as electric automobile for cycle performance of battery and thermal stability at main equipment, therefore there is in recent years good cycling stability, chemical stability is good, the lithium iron phosphate cathode material of the many advantages such as Heat stability is good gets the attention and studies, and LiFePO 4 also has the high (170mAhg of theoretical capacity
-1), low production cost and the advantage such as nontoxic.
But FeO in the LiFePO 4 structure
6the octahedra oxygen atom that shares, form the octahedral structure on summit altogether, and this structure has caused the LiFePO 4 conductivity very low by (10
-9～10
-11scm
-1); In LiFePO 4, the lithium ion migrating channels is one-dimentional structure in addition, and this also causes its lithium ion mobility low.The two causes the electric conductivity of lithium iron phosphate cathode material not good jointly, and capacity is very fast with charge-discharge magnification raising decay.The main path addressed this problem at present is adulterate (being mainly carbon film coated) and reduce the mode of material granule size by amorphous phase.Wherein, the amorphous phase doping can significantly improve the conductivity (10 of material
-3～10
-1scm
-1); And particle size reduce to have shortened the lithium ion migration distance, thereby improved the lithium ion mobility.
The method for preparing the nano-lithium iron phosphate of carbon coating has solid phase method or liquid phase method.Wherein liquid phase method is first prepared LiFePO 4, and afterwards dry and carbon source is carried out ball milling and completed carbon coating, finally high-temperature roasting under atmosphere of inert gases.The LiFePO 4 particle diameter that liquid phase method obtains is less, but ball-milling method is difficult to guarantee that carbon film evenly is coated on the LiFePO 4 particle surface, and follow-up high-temperature calcination process also weakened the low advantage of liquid phase method energy consumption, complicated technological process also is unfavorable for its application aborning in addition.Therefore, the suitability for industrialized production LiFePO 4 is mainly used solid phase method at present, and LiFePO 4 preparation and carbon film coated one step complete.In the solid phase reaction process traditional, various solid reactants are difficult to mix, and all need to carry out high strength in raw material preparatory stage and course of reaction, grind for a long time, and whole preparation time often reached more than 30 hours.Both just like this; the character such as the purity of gained positive electrode and granularity are still inhomogeneous; show that granularity reaches sub-micron to micron level and particle diameter and distributes wide; carbon film coated is inhomogeneous; the quality conformance of different batches product is poor, and these have all had a strong impact on large-scale production and the application of ferrousphosphate lithium material.The technology of preparing that develops the nanometer ferrousphosphate lithium material of even carbon coating is the important topic of academia and industrial circle extensive concern.
Summary of the invention
In order to address the above problem, the present invention proposes the method that solid phase method prepares the nano-lithium iron phosphate of even carbon coating.Nano ferric phosphate and nanoscale lithium-containing compound and carbon source form the homodisperse fluid of receiving by solvent, then the solvent of receiving in fluid by fast eliminatings such as spray-on processes, have obtained the solid mixture that phosphorus source, source of iron, lithium source, carbon source mix; Do reactant with this solid mixture mixed, improved mass transfer rate and the controllability of solid phase method process, thereby can obtain the nano-lithium iron phosphate particle that even carbon coats.
A kind of method for preparing the nano-lithium iron phosphate of carbon coating, realize by following steps:
1) according to mol ratio Fe: Li: C, (iron: lithium: carbon)=1: 1: the ratio of (1～5) is got nano ferric phosphate, nanometer lithium salts and carbon source, again by its dissolving or be distributed in solvent the fluid of receiving that obtains stable uniform, then the solvent that will receive in fluid removes rapidly, the solid particulate reagent be uniformly mixed;
2), in atmosphere of hydrogen, atmosphere of inert gases or hydrogen and inert gas mist atmosphere, the above-mentioned mixed uniformly solid particulate reagent of roasting (through certain heating schedule, completing solid phase reaction), obtain the nano-lithium iron phosphate that carbon coats.Products obtained therefrom is the nano-lithium iron phosphate that even carbon coats.
The particle size range 10-200nm of described nano ferric phosphate.
Described nanometer lithium salts is one or more in lithium carbonate, lithium hydroxide, lithium dihydrogen phosphate or their hydrate.
Described carbon source is one or more in glucose, citric acid, oxalic acid, stearic acid, vitamin C, acetylene black or carbon nano-tube.
The described fluid solvent of receiving is one or more in water, ethanol, isopropyl alcohol or acetone.
The described dispersing mode that obtains receiving fluid is one or more in ball mill grinding, ultrasonic or bubbling.
It is described that to remove the method for solvent in fluid of receiving be one or more in spray drying, vacuumize, flash distillation or freeze-day with constant temperature.
The preferred argon atmosphere of described atmosphere of inert gases, in hydrogen and inert gas mist atmosphere, the shared percent by volume of hydrogen is less than or equal to 5% for being greater than zero.
Roasting reactor used is tubular react furnace or Muffle furnace.
Described roasting is in the following way: first 200-400 ℃ of preroast 1-3h, 500-800 ℃ of roasting 5-12h then, wherein, during roasting, heat up with the heating rate of 2-10K/min.
Beneficial effect of the present invention is:
Be different from liquid/vapor, in solid phase, diffusion coefficient is than low 4-5 more than the order of magnitude in gas phase or liquid phase, so solid phase reaction is the mass transport limitation process substantially.The rising temperature can improve diffusion coefficient, and therefore most of solid phase reactions need at high temperature be carried out.Except diffusion coefficient, mass transfer distance has also determined diffusion rate, it is generally acknowledged square being inversely proportional to of diffusion time and diffusion length.In the present invention, use nano raw material to do reactant, this has just shortened the mass transfer distance, thereby makes to shorten diffusion time 1-2 more than the order of magnitude, has also shortened the solid phase reaction required time when promoting mass transfer.
In addition, in solid phase, extremely low diffusion coefficient makes the microcosmic admixture of solid reactant become the key factor of reaction.When solid reactant mixes when inhomogeneous, not mating of regional area reactant stoichiometric proportion can cause reaction not carry out fully, and side reaction even occurs.In tradition solid phase reaction process with ball mill by within several hours, having ground the abundant mixing of solid reactant.Whole process not only of long duration, energy consumption is high, and the compound particles particle diameter obtained distributes wide.The present invention forms the stable fluid of receiving by the nanometer presoma being placed in to solvent and fully disperseing, and then removes rapidly the solvent received in fluid to obtain the solid mixture of homogeneous, and mixed method is simple, quick, effective, energy-conservation.The particle diameter of the carbon cladded ferrous lithium phosphate that the present invention prepares is 30-500nm, and particle size distribution is more even.
Preparation method's production efficiency that the present invention proposes is high, easy to implement, and the grain diameter of the carbon cladded ferrous lithium phosphate obtained is at nanoscale, narrowly distributing, and carbon film is even, contributes to improve ionic mobility and conductivity, improves the consistency of anode material for lithium-ion batteries.
The accompanying drawing explanation
Fig. 1 is transmission electron microscope (TEM) figure of the nanometer presoma that uses of the embodiment of the present invention 1.Wherein, (a) being nano ferric phosphate SEM figure, is (b) nano lithium carbonate TEM figure.
Fig. 2 is transmission electron microscope (TEM) and ESEM (SEM) figure of the prepared sample A of the embodiment of the present invention 1.
Fig. 3 is the XRD collection of illustrative plates of the prepared sample A of the embodiment of the present invention 1.
Embodiment
The following examples can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.
Embodiment 1
1) according to mol ratio Fe: Li: C=1: the ratio of 1: 2.5 is got nano ferric phosphate, nano lithium carbonate and stearic acid, and wherein ferric phosphate is got 0.005mol.Stearic acid is dissolved in ethanol, and then adds wherein nano ferric phosphate and nano lithium carbonate.By the ultrasonic 15min of gained suspension-turbid liquid, obtain the fluid of receiving of stable uniform.The fluid of receiving is placed in 80 ℃ of dry 30min of constant temperature oven, obtains the solid particle reactant mixture after desolvation.
2) gained solid particle reactant mixture is placed in to tubular react furnace, 300 ℃ of preroast 1h in inert gas Ar atmosphere is enclosed, 700 ℃ of roasting 6h, wherein, heating rate 5K/min.Naturally obtain the LiFePO 4 particle after cooling, be designated as sample A.
Fig. 1 is nano ferric phosphate SEM figure and the nano lithium carbonate TEM figure that embodiment 1 is used, and can find out that two kinds of nanometer presoma particle diameters are respectively 100nm and 50nm, and all has narrow particle diameter distribution.The XRD collection of illustrative plates that Fig. 2 is the sample A for preparing of embodiment 1, prove that it is olivine-type structure and free from admixture.The SEM photo that Fig. 3 is the sample A for preparing of embodiment 1, can find out that grain diameter is the 100nm left and right.
Embodiment 2
1) according to mol ratio Fe: Li: C=1: the ratio of 1: 5 is got nano ferric phosphate, nano lithium carbonate and vitamin C, and wherein ferric phosphate is got 0.005mol.Vitamin C is dissolved in the aqueous acetone solution containing acetone 50%, and then adds wherein nano ferric phosphate and nano lithium carbonate.By the ultrasonic 15min of gained suspension-turbid liquid, obtain the fluid of receiving of stable uniform.The fluid of receiving is sent into the vacuum desiccator desolvation, obtains the solid particle reactant mixture.
2) gained solid particle reactant mixture is placed in to tubular react furnace, 300 ℃ of preroast 1h in inert gas Ar atmosphere is enclosed, 700 ℃ of roasting 6h, wherein, heating rate 5K/min.Naturally obtain the LiFePO 4 particle after cooling.
Embodiment 3
1) according to mol ratio Fe: Li: C=1: the ratio of 1: 3 is got nano ferric phosphate, nano lithium carbonate and oxalic acid, and wherein ferric phosphate is got 0.005mol.Oxalic acid is dissolved in the isopropanol water solution containing isopropyl alcohol 30%, and then adds wherein nano ferric phosphate and nano lithium carbonate.By gained suspension-turbid liquid mechanical lapping 15min, obtain the fluid of receiving of stable uniform.The fluid of receiving is sent into desolvation in flash vessel, obtains the solid particle reactant mixture.
2) gained solid particle reactant mixture is placed in to tubular react furnace, 300 ℃ of preroast 1h in atmosphere of hydrogen, 700 ℃ of roasting 6h, wherein, heating rate 10K/min.Naturally obtain the LiFePO 4 particle after cooling.
Embodiment 4
1) according to mol ratio Fe: Li: C=1: the ratio of 1: 4 is got nano ferric phosphate, nano lithium carbonate and glucose, and wherein ferric phosphate is got 0.005mol.Glucose is soluble in water, and then add wherein nano ferric phosphate and nano lithium carbonate.To gained suspension-turbid liquid bubbling 60min, obtain the fluid of receiving of stable uniform.The fluid of receiving is sent into the thermostatic drying chamber desolvation, obtains the solid particle reactant mixture.
2) gained solid particle reactant mixture is placed in to tubular react furnace, in the mist atmosphere of hydrogen and inert gas argon gas, wherein the shared percent by volume of hydrogen is 5%, 300 ℃ of preroast 3h, 700 ℃ of roasting 12h, wherein, heating rate 5K/min.Naturally obtain the LiFePO 4 particle after cooling.
Embodiment 5
1) according to mol ratio Fe: Li: C=1: the ratio of 1: 2.5 is got nano ferric phosphate, nano lithium carbonate and acetylene black, and wherein ferric phosphate is got 0.005mol.Acetylene black, nano ferric phosphate are put into to ethanol together with nano lithium carbonate, by the ultrasonic 15min of gained suspension-turbid liquid, obtain the fluid of receiving of stable uniform.The fluid of receiving is placed in 80 ℃ of dry 30min of constant temperature oven, obtains the solid particle reactant mixture after desolvation.
2) gained solid particle reactant mixture is placed in to tubular react furnace, in the mist atmosphere of hydrogen and inert gas helium, wherein the shared percent by volume of hydrogen is 3%, 300 ℃ of preroast 1h, 700 ℃ of roasting 6h, wherein, heating rate 5K/min.Naturally obtain the LiFePO 4 particle after cooling.
Embodiment 6
1) according to mol ratio Fe: Li: C=1: the ratio of 1: 1 is got nano ferric phosphate, nano lithium carbonate and carbon nano-tube, and wherein ferric phosphate is got 0.005mol.Carbon nano-tube, nano ferric phosphate are put into to acetone together with the nano lithium carbonate body, by the ultrasonic 15min of gained suspension-turbid liquid, obtain the fluid of receiving of stable uniform.The fluid of receiving is placed in 80 ℃ of dry 30min of constant temperature oven, obtains the solid particle reactant mixture after desolvation.
2) gained solid particle reactant mixture is placed in to tubular react furnace, 300 ℃ of preroast 1h in the inert gas argon atmospher is enclosed, 700 ℃ of roasting 6h, wherein, heating rate 5K/min.Naturally obtain the LiFePO 4 particle after cooling.
Embodiment 7
1) according to mol ratio Fe: Li: C=1: the ratio of 1: 2.5 is got nano ferric phosphate, lithium dihydrogen phosphate and stearic acid, and wherein ferric phosphate is got 0.005mol.Stearic acid is dissolved in acetone, then nano ferric phosphate and lithium dihydrogen phosphate is placed in to acetone.By the ultrasonic 15min of gained suspension-turbid liquid, obtain the fluid of receiving of stable uniform.The fluid of receiving is placed in 80 ℃ of dry 30min of constant temperature oven, obtains the solid particle reactant mixture after desolvation.
2) gained solid particle reactant mixture is placed in to tubular react furnace, 200 ℃ of preroast 3h in the inert gas argon atmospher is enclosed, 800 ℃ of roasting 12h, wherein, heating rate 2K/min.Naturally obtain the LiFePO 4 particle after cooling.
Embodiment 8
1) according to mol ratio Fe: Li: C=1: the ratio of 1: 2.5 is got nano ferric phosphate, nano lithium carbonate and stearic acid, and wherein ferric phosphate is got 0.005mol.Stearic acid is dissolved in the acetone-ethanolic solution containing acetone 50%, and then nano ferric phosphate and nano lithium carbonate are added to solution.By the ultrasonic 15min of gained suspension-turbid liquid, obtain the fluid of receiving of stable uniform.The fluid of receiving is placed in 80 ℃ of dry 30min of constant temperature oven, obtains the solid particle reactant mixture after desolvation.
2) gained solid particle reactant mixture is placed in to Muffle furnace, 400 ℃ of preroast 1h in the inert gas argon atmospher is enclosed, 800 ℃ of roasting 5h, wherein, heating rate 10K/min.Naturally obtain the LiFePO 4 particle after cooling.
Embodiment 9
1) according to mol ratio Fe: Li: C=1: the ratio of 1: 2.5 is got nano ferric phosphate, nano lithium carbonate and stearic acid, and wherein ferric phosphate is got 0.005mol.Stearic acid is dissolved in ethanol, and then nano ferric phosphate and nano lithium carbonate are added to solution.By gained suspension-turbid liquid ball mill grinding 15min, obtain the fluid of receiving of stable uniform.The fluid of receiving is placed in the dry 30min of vacuum drying chamber, obtains the solid particle reactant mixture after desolvation.
2) gained solid particle reactant mixture is placed in to Muffle furnace, 300 ℃ of preroast 1h in the inert gas argon atmospher is enclosed, 700 ℃ of roasting 6h, wherein, heating rate 10K/min.Naturally obtain the LiFePO 4 particle after cooling.
Embodiment 10
1) according to mol ratio Fe: Li: C=1: the ratio of 1: 5 is got nano ferric phosphate, nanometer lithium hydroxide and acetylene black, and wherein ferric phosphate is got 0.005mol.Acetylene black, nano ferric phosphate are put into to ethanol together with the nanometer lithium hydroxide, by the ultrasonic 15min of gained suspension-turbid liquid, obtain the fluid of receiving of stable uniform.The fluid of receiving is placed in 80 ℃ of dry 30min of constant temperature oven, obtains the solid particle reactant mixture after desolvation
2) gained solid particle reactant mixture is placed in to Muffle furnace, 300 ℃ of preroast 2h in the inert gas argon atmospher is enclosed, 700 ℃ of roasting 12h, wherein, heating rate 10K/min.Naturally obtain the LiFePO 4 particle after cooling.
The above; be only the present invention's embodiment preferably, but protection scope of the present invention is not limited to this, anyly is familiar with in technical scope that those skilled in the art disclose in the present invention; the variation that can expect easily or replacement, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection range of claim.
Claims (5)
1. a method for preparing the nano-lithium iron phosphate that carbon coats is characterized in that: by following steps, realize:
1) according to mol ratio Fe:Li:C=1:1:(1～5) ratio get nano ferric phosphate, nanometer lithium salts and carbon source, again by its dissolving or be distributed in solvent the fluid of receiving that obtains stable uniform, then the solvent that will receive in fluid removes rapidly, the solid particulate reagent be uniformly mixed;
2), in atmosphere of hydrogen, atmosphere of inert gases or hydrogen and inert gas mist atmosphere, the above-mentioned mixed uniformly solid particulate reagent of roasting, obtain the nano-lithium iron phosphate that carbon coats;
The particle size range 10-200nm of described nano ferric phosphate;
Described nanometer lithium salts is one or more in lithium carbonate, lithium hydroxide, lithium dihydrogen phosphate or their hydrate;
Described carbon source is one or more in glucose, citric acid, oxalic acid, stearic acid, vitamin C, acetylene black or carbon nano-tube;
The described fluid solvent of receiving is one or more in water, ethanol, isopropyl alcohol or acetone;
Described roasting is in the following way: first 200-400 ℃ of preroast 1-3h, 500-800 ℃ of roasting 5-12h then, wherein, during roasting, heat up with the heating rate of 2-10K/min.
2. method according to claim 1 is characterized in that: the described dispersing mode that obtains receiving fluid is one or more in ball mill grinding, ultrasonic or bubbling.
3. method according to claim 1 is characterized in that: described to remove the method for solvent in fluid of receiving be one or more in spray drying, vacuumize, flash distillation or freeze-day with constant temperature.
4. method according to claim 1 is characterized in that: in described hydrogen and inert gas mist atmosphere, the shared percent by volume of hydrogen is less than or equal to 5% for being greater than zero.
5. method according to claim 1, it is characterized in that: roasting reactor used is tubular react furnace or Muffle furnace.
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| CN105655548A (en) * | 2014-12-03 | 2016-06-08 | 中国电子科技集团公司第十八研究所 | Method for uniform carbon coating on lithium iron phosphate surface |
| CN104591113B (en) * | 2014-12-28 | 2017-02-22 | 山东精工电子科技有限公司 | Low-temperature lithium iron phosphate positive pole material capable of implementing uniform coating preparation by modification flash distillation plant and preparation method thereof |
| CN106563433B (en) * | 2016-11-15 | 2019-02-26 | 电子科技大学 | A kind of carbon-coated TiO2Material and preparation method thereof |
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|---|---|---|---|---|
| CN101330141A (en) * | 2008-07-18 | 2008-12-24 | 清华大学 | Method for preparing lithium ionic battery anode material spherical LiFePO4 /C |
| CN101693531A (en) * | 2009-10-16 | 2010-04-14 | 清华大学 | Method for preparing nano iron phosphate |
| CN101901899A (en) * | 2009-12-07 | 2010-12-01 | 耿世达 | Nano lithium iron phosphate material for lithium battery anode and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101330141A (en) * | 2008-07-18 | 2008-12-24 | 清华大学 | Method for preparing lithium ionic battery anode material spherical LiFePO4 /C |
| CN101693531A (en) * | 2009-10-16 | 2010-04-14 | 清华大学 | Method for preparing nano iron phosphate |
| CN101901899A (en) * | 2009-12-07 | 2010-12-01 | 耿世达 | Nano lithium iron phosphate material for lithium battery anode and manufacturing method thereof |
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