CN102097616A - Preparation method of high-energy and high-power density nano-scale lithium iron phosphate powder - Google Patents
Preparation method of high-energy and high-power density nano-scale lithium iron phosphate powder Download PDFInfo
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- CN102097616A CN102097616A CN2011100045066A CN201110004506A CN102097616A CN 102097616 A CN102097616 A CN 102097616A CN 2011100045066 A CN2011100045066 A CN 2011100045066A CN 201110004506 A CN201110004506 A CN 201110004506A CN 102097616 A CN102097616 A CN 102097616A
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Abstract
The invention provides a preparation method of a nano-scale lithium iron phosphate powder. The method comprises the following steps: a. preparing a precursor through an improved sol-gel method; b. drying the gel prepared in the step a at the temperature of 60-90 DEG C; and c. transferring the product of the step b into an atmosphere furnace, heating to 500-800 DEG C at a heating rate of 1-20 DEG C/min under the inert or weak reducing atmosphere, sintering for 8-25 hours at constant temperature and crushing after cooling so as to obtain the high-energy density and high-power density spherical nano-scale lithium iron phosphate powder. The preparation method has the advantages of simple preparation process, few controllable factors, short production cycle, low cost and energy consumption and good repeatability, and is applicable to industrialized production. Used raw materials are all cheap, non-toxic and pollution-free inorganic compounds. The prepared powder has the advantages of good uniformity, high purity and controlled granularity and appearance.
Description
Technical field
The present invention relates to the technical field of electrochemical energy storage power, particularly the preparation method of high-energy, high power density type lithium iron phosphate nano powder.Prepared spheroidization, Nano level powder of lithium iron phosphate can be used for various types of lithium ion batteries and ultracapacitor, are specially adapted to the power-type lithium ion battery system.
Background technology
The development of the portable electric appts of miniaturization, multifunction has driven the deep development of the removable energy in the whole world comprehensively and has updated; The development of Aero-Space and national defence hard-core technology equipment has also proposed the requirement of aspects such as high-performance, high security to the removable energy; The speed of exploitation high efficient energy sources memory devices has been accelerated in the aggravation of oil crisis and the deterioration of environment especially.Lithium ion battery is as high efficient energy sources memory device of new generation, have that operating voltage height, volume are little, light weight, specific energy height, self discharge are little, memory-less effect, have extended cycle life, plurality of advantages such as operating temperature range height.At present, can the energy storage secondary lithium battery system that break through cheapness, safety, green non-pollution, excellent performance have become from now on one of material technical field of tool in the development of world economy.The raising that the widening of the lifting of lithium ion battery performance and range of application depended on the positive electrode performance to a great extent and the decline of cost, therefore, exploitation performance and price become the emphasis of Study on Li-ion batteries using than all good positive electrodes.
At present, commercial anode material for lithium-ion batteries is mainly based on cobalt acid lithium.Although this kind material has good stable, high voltage, high advantages such as specific capacity, but the raw material costliness of synthetic this kind positive electrode, contaminated environment, the high high-temp stability of this kind material is poor simultaneously, fail safe is not good, and these deficiencies have greatly limited the large-scale application of this kind material.In the numerous anode material for lithium-ion batteries that occur in succession, LiFePO4 has low cost, aboundresources, non-environmental-pollution, theoretical capacity is higher, charge and discharge platform is mild, and the life-span is long, advantages such as Heat stability is good, be considered to tool development potentiality, safest anode material for lithium-ion batteries, especially be considered to the preferred material that great-capacity power battery is used.
But as the anode material for lithium-ion batteries of new generation of tool potentiality to be exploited and application prospect, in synthetic and practicability, mainly there is following problem as previously mentioned:
1, batch stability of product is not good.At present, the synthetic method that can realize volume production both at home and abroad is mainly high-temperature solid phase reaction method and carbothermic method.High-temperature solid phase reaction method normally adopts the mode of grinding to carry out the mixing of material, but grinds the uniformity that batch mixing is difficult to guarantee chemical composition, the not enough problem of product batches stability therefore can occur.Meanwhile, the product particle of solid phase reaction is thick, and particle size distribution is wider, and chemical property is relatively poor.It is source of iron that carbothermic method generally adopts trivalent iron salt, sintering LiFePO4 under high temperature and inert atmosphere, but the addition of synthesis temperature and carbon is wayward.Temperature is low excessively, and the addition of carbon is very few, and ferric iron can not be reduced to ferrous iron fully; Temperature is too high, and the addition of carbon is too much, has fe or iron phosphide and generates.
2, raw material and production route are lacked competitiveness.Adopt hydro thermal method and microwave sintering method can obtain pure LiFePO4, very harsh but this synthetic method requires process conditions, and need special production equipment, therefore be difficult to realize large-scale production.Sol-gel process is a kind of synthesizing to have the method for high electrochemical activity lithium iron phosphate positive material, and this method can guarantee the high-purity and the high homogeneity of product, can effectively control microstructure of product from the synthetic initial period.But; there are shortcomings such as production cycle length, synthesis technique more complicated, governing factor are many in existing sol-gel process; have at least a kind of raw material to be expensive and the poisonous organic alkoxide of metal in the raw material combination that is adopted simultaneously, these deficiencies have greatly limited the scale of this method and have used.
Summary of the invention
The objective of the invention is to improve the deficiency of existing sol-gel process, provide a kind of with cheap, nontoxic, free of contamination inorganic compound be combined as raw material, preparation has a method of high-energy and high power density nano ferric phosphate powder for lithium, this preparation method's technology is simple, controllable factor is few, with short production cycle, cost and energy consumption are low, is highly susceptible to industrialized implementation.The granularity and the pattern of the nano ferric phosphate powder for lithium of this method preparation are controlled, and environmental protection.
The preparation method of high-energy of the present invention, high power density type nano ferric phosphate powder for lithium may further comprise the steps:
A. the sol-gel process with improvement prepares presoma:
By amount of substance, lithium source, source of iron and the phosphorus source of Li: Fe: P=0.9～12: 1: 1 joined respectively in the organic solvent fully stir, question response fully after, add a certain amount of conductive materials predecessor, at room temperature make colloidal sol, leave standstill then and make colloidal sol change gel into; Wherein, source of iron is at least a in the inorganic compound group formed of frerrous chloride, iron chloride, ferrous oxide, iron oxide, iron hydroxide, ferric phosphate and ferrous carbonate, and lithium source and phosphorus source are cheap, nontoxic, free of contamination inorganic compound or its mixture;
B. the gel that step a is made places and carries out dried under 60～90 ℃;
C. the product with step b changes in the atmosphere furnace, under inertia or weakly reducing atmosphere, heating rate with 1～20 ℃/min is heated to 500～800 ℃, constant temperature sintering 8～25h, broken spheroidization, the Nano level powder of lithium iron phosphate that promptly obtains having high-energy-density and high power density in cooling back.
Described step b can also comprise a presintering operation, this presintering operation comprises: with the product after the dried among the step b under inertia or weakly reducing atmosphere, heating rate with 1～20 ℃/min is heated to 250～400 ℃, and constant temperature sintering 3～10h is broken after cooling.
Step b can also comprise a granulating working procedure after the presintering operation, with aggregate particle size (10～1 μ m) and the pattern (sphere) of controlling product more effectively, this granulating working procedure comprises: the product that also passes through break process after the step b presintering is scattered in a certain amount of water, absolute ethyl alcohol or other organic solvents, carries out spray drying treatment.
In the said method, the coating of nano-carbon film and the preparation of precursor are carried out in the lump, do not need extra carbon to coat operation.
At least a in the inorganic compound group that the preferred lithium chloride in described lithium source, lithium hydroxide, lithium carbonate, lithium phosphate and lithium dihydrogen phosphate are formed; At least a in the inorganic compound group that described phosphorus source preferably phosphoric acid lithium, lithium dihydrogen phosphate, phosphoric acid and phosphorus pentoxide are formed.Can arrange in pairs or groups arbitrarily and make up between described source of iron, lithium source and the phosphorus source.
At least a in the preferred glucose of described conductive materials predecessor, citric acid, laurate, sucrose, vitamin C, oxalic acid and the softex kw.
At least a in the preferred isopropyl alcohol of the described organic solvent of step a, ethylene glycol, ethanol and the isooctane.
The gaseous mixture of described inertia or the preferred argon gas of weak reducing gas or nitrogen or argon body and hydrogen or the gaseous mixture of nitrogen and hydrogen.
The addition of the predecessor of conductive materials described in the step a is preferably: it is 1% (weight)～6% (weight) that the conductive materials predecessor that is added can make the remaining carbon of the LiFePO4 that makes.
Can also utilize again solvent recovery by solvent recovering system.
The present invention has the following advantages:
1, the present invention adopts the synthetic presoma of sol-gel process of improvement, and synthesis technique is simple, and is with short production cycle, and controllable factor is few, easy operating.
2, used lithium source, source of iron and the phosphorus source of the present invention is cheapness, nontoxic, free of contamination inorganic compound or its mixture.
3, the powder good uniformity that adopts the present invention to make, the purity height, granularity and pattern are controlled, favorable repeatability.
4, the synthetic of carbon coating processing and presoma finished in the lump among the present invention, and guaranteed the even coating of nano-carbon film.
5, adopt the LiFePO 4 material charge/discharge capacity height of the present invention's preparation, high rate performance is superior, good cycling stability.When the addition of conductive agent was 5wt%, in the voltage range of 2.3～4.5V, the specific discharge capacity of 0.1C was about 162mAh/g, and the specific discharge capacity of 5C is about 120mAh/g, and the specific discharge capacity of 10C reaches 110mAh/g.
Compared with prior art, preparation technology of the present invention is simple, and controllable factor is few, and is with short production cycle, and cost and energy consumption are low, and favorable repeatability is applicable to suitability for industrialized production.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the energy density type nano ferric phosphate powder for lithium of embodiment 1-3 preparation.
Fig. 2 is the electron scanning micrograph of the energy density type nano ferric phosphate powder for lithium of embodiment 1 preparation.
Fig. 3 is the specific discharge capacity figure of energy energy density type nano ferric phosphate powder for lithium under different charge-discharge magnifications of embodiment 1 preparation.
Fig. 4 is the electron scanning micrograph of the energy density type nano ferric phosphate powder for lithium of embodiment 2 preparations.
Fig. 5 is the specific discharge capacity figure of energy density type nano ferric phosphate powder for lithium under the 1C multiplying power of embodiment 2 preparations.
Fig. 6 is the specific discharge capacity figure of energy density type nano ferric phosphate powder for lithium under the 1C multiplying power of embodiment 3 preparations.
Embodiment
The present invention will be further described below in conjunction with specific embodiment and accompanying drawing.
Embodiment 1:
By amount of substance, with Li: Fe: P=1: 1: 1 lithium carbonate, four water frerrous chlorides and phosphoric acid join respectively in a certain amount of absolute ethyl alcohol, mix, after question response is complete, according to the remaining carbon of final LiFePO4 is that the amount of 4.5% (weight) adds corresponding citric acid, makes its whole dissolvings, stirs, at room temperature place, colloidal sol is converted into gel;
The gel that makes is placed 85 ℃ of dryings down, change over to then in the atmosphere furnace, in argon atmospher, that xerogel is at 350 ℃ of following presintering 5h, broken behind the natural cooling;
The presintering product is changed in the atmosphere furnace, under argon atmospher,, promptly get energy density type nano ferric phosphate powder for lithium behind the natural cooling at 650 ℃ of following sintering 15h.
The X ray diffracting spectrum of the energy density type nano ferric phosphate powder for lithium that embodiment 1 makes as shown in Figure 1, the nano ferric phosphate powder for lithium that embodiment 1 makes is the olivine-type LiFePO 4 powder of pure phase, and the crystal property of product is good.
Figure 2 shows that the electron scanning micrograph of the energy density type nano ferric phosphate powder for lithium that embodiment 1 makes, as can be seen, the LiFePO4 that embodiment 1 makes is spheroidization, nanometer grade powder, and the particle mean size of product is that particle size distribution is narrower about 70 nanometers.
By weight, LiFePO 4 powder, 5% conductive agent and 5% binding agent that 90% embodiment 1 is made are dispersed in the N-methyl pyrrolidone, be modulated into mobile suitable slurry, and evenly be coated on the aluminium foil, make anode pole piece to be measured through steps such as oven dry, sections.With the metal lithium sheet is negative pole, the lithium hexafluoro phosphate solution of the ethylene carbonate of 1M and diethyl carbonate (volume ratio 1: 1) is electrolyte, Celgard 2500 is a barrier film, is assembled into button cell the chemical property of lithium iron phosphate positive material is tested and assessed.
Test result, the high rate performance of the energy density type nano ferric phosphate powder for lithium that embodiment 1 makes as shown in Figure 3.In the voltage range of 2.3～4.5V, the specific discharge capacity of 0.1C reaches 162mAh/g, and the specific discharge capacity of 5C is about 120mAh/g, and the 10C specific discharge capacity is about 110mAh/g.Along with the growth of cycle-index, specific capacity remains unchanged substantially, illustrates that the cyclical stability of this material is good.
Embodiment 2:
By amount of substance, take by weighing Li: Fe=12: 1 lithium dihydrogen phosphate and four water frerrous chlorides, they are joined respectively in a certain amount of isopropyl alcohol, stir, after question response is complete, remaining carbon according to final LiFePO4 is that 2.3% (weight) adds required citric acid, and it is dissolved fully, at room temperature places and promptly gets required gel;
The gel that makes is placed 60 ℃ of dryings down, change over to after the drying in the atmosphere furnace, in argon atmospher,, broken behind the natural cooling at 400 ℃ of following presintering 6h;
The presintering product is changed in the atmosphere furnace, in argon atmospher,, promptly get energy density type nano ferric phosphate powder for lithium behind the natural cooling at 650 ℃ of following sintering 10h.
The XRD figure spectrum of the nano ferric phosphate powder for lithium that embodiment 2 makes as shown in Figure 1.The crystal structure diffracting spectrum shows that embodiment 2 has prepared the olivine-type LiFePO 4 powder of single phase.The electron scanning micrograph of the LiFePO 4 powder that Fig. 4 makes for embodiment 2, as can be seen, the granularity of product LiFePO 4 powder is approximately 80 nanometers, narrow diameter distribution.
Press the method for testing of embodiment 1, the nano ferric phosphate powder for lithium that embodiment 2 makes is made anode pole piece to be measured, and then carry out electrochemical property test after being assembled into button cell.Test result as shown in Figure 5, as can be seen, with the 1C rate charge-discharge, specific discharge capacity first is 140mAh/g, circulates after 100 times, capacity remains unchanged substantially, has embodied excellent cyclical stability.
Embodiment 3:
By amount of substance, with Li: Fe: P=1: 1: 1 lithium carbonate, iron chloride and ammonium phosphate add respectively in the mixed liquor of ethylene glycol and absolute ethyl alcohol, fully stir, after question response is complete, add proper vitamin C, treat that it dissolves fully, promptly get required colloidal sol, at room temperature place gel;
This gel is placed 90 ℃ of dryings down, promptly get xerogel;
This xerogel is moved in the atmosphere furnace, in 95V% argon gas and 5V% hydrogen mixed gas, be heated to 300 ℃, constant temperature presintering 5h, broken behind the natural cooling;
Product after the presintering is moved in the atmosphere furnace, in 95V% argon gas and 5V% hydrogen mixed gas, be heated to 600 ℃, constant temperature sintering 20h promptly gets energy density type nano ferric phosphate powder for lithium behind the natural cooling.
The XRD figure spectrum of the nano ferric phosphate powder for lithium product that embodiment 3 makes as shown in Figure 1.As seen from the figure, embodiment 3 has prepared the olivine-type LiFePO 4 powder of pure phase.
Press the method for testing of embodiment 1, the nano ferric phosphate powder for lithium that embodiment 3 makes is made anode pole piece to be measured, and then carry out electrochemical property test after being assembled into button cell.Test result as shown in Figure 6, as can be seen, with the 1C rate charge-discharge, specific discharge capacity first is 123mAh/g, circulates after 100 times, capacity remains unchanged substantially, has embodied excellent cyclical stability.
Except that above embodiment, the present invention can also list more embodiment by the following technical solutions.As, Li source compound can also be selected from lithium hydroxide, lithium chloride or lithium phosphate, and Fe source compound can also be selected from iron oxide, ferrous oxide, iron hydroxide or ferric phosphate, and P source compound can be selected from ammonium hydrogen phosphate, ammonium dihydrogen phosphate or lithium phosphate.
The invention is not restricted to this, any based on of the present invention substitute and modify all should be included in, protection scope of the present invention is as the criterion with claims.
Claims (9)
1. the preparation method of a nano ferric phosphate powder for lithium is characterized in that may further comprise the steps:
A. the sol-gel process with improvement prepares presoma:
By amount of substance, lithium source, source of iron and the phosphorus source of Li: Fe: P=0.9～1.2: 1: 1 joined respectively in the organic solvent fully stir, question response fully after, add a certain amount of conductive materials predecessor, at room temperature make colloidal sol, leave standstill then and make colloidal sol change gel into; Wherein, source of iron is at least a in the inorganic compound group formed of frerrous chloride, iron chloride, ferrous oxide, iron oxide, iron hydroxide, ferric phosphate and ferrous carbonate, and lithium source and phosphorus source are cheap, nontoxic, free of contamination inorganic compound or its mixture;
B. the gel that step a is made places and carries out dried under 60～90 ℃;
C. the product with step b changes in the atmosphere furnace, under inertia or weakly reducing atmosphere, heating rate with 1～20 ℃/min is heated to 500～800 ℃, constant temperature sintering 8～25h, broken spheroidization, the Nano level powder of lithium iron phosphate that promptly obtains having high-energy-density and high power density in cooling back.
2. preparation method according to claim 1, it is characterized in that, described step b also comprises a presintering operation, this presintering operation comprises: with the product after the dried among the step b under inertia or weakly reducing atmosphere, heating rate with 1～20 ℃/min is heated to 250～400 ℃, constant temperature sintering 3～10h, broken after cooling.
3. preparation method according to claim 2, it is characterized in that, described step b also comprises a granulating working procedure, this granulating working procedure comprises: the product that also passes through break process after the step b presintering is scattered in a certain amount of water, absolute ethyl alcohol or other organic solvents, carries out spray drying treatment.
4. preparation method according to claim 1 is characterized in that: the coating of nano-carbon film and the preparation of precursor are carried out in the lump, do not need extra carbon to coat operation.
5. according to each described preparation method among the claim 1-4, it is characterized in that: described lithium source is at least a in the inorganic compound group formed of lithium chloride, lithium hydroxide, lithium carbonate, lithium phosphate and lithium dihydrogen phosphate; Described phosphorus source is at least a in the inorganic compound group formed of lithium phosphate, lithium dihydrogen phosphate, phosphoric acid and phosphorus pentoxide.
6. according to each described preparation method among the claim 1-4, it is characterized in that: described conductive materials predecessor is at least a in glucose, citric acid, laurate, sucrose, vitamin C, oxalic acid and the softex kw.
7. according to each described preparation method among the claim 1-4, it is characterized in that: the described organic solvent of step a is at least a in isopropyl alcohol, ethylene glycol, ethanol and the isooctane.
8. according to each described preparation method among the claim 1-4, it is characterized in that: described inertia or weak reducing gas are the gaseous mixture of argon gas or nitrogen or argon body and hydrogen or the gaseous mixture of nitrogen and hydrogen.
9. according to each described preparation method among the claim 1-4, it is characterized in that the addition of the predecessor of conductive materials described in the step a is defined as: it is 1% (weight)～6% (weight) that the conductive materials predecessor that is added can make the remaining carbon of the LiFePO4 that makes.
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| CN102496714A (en) * | 2011-12-27 | 2012-06-13 | 天津力神电池股份有限公司 | Anode active substance, production method thereof, and lithium ion battery employing anode active substance |
| CN102491426A (en) * | 2011-12-09 | 2012-06-13 | 东莞市迈科科技有限公司 | Preparation method for lithium battery anode material LiNi0.5Mn1.5O4 |
| CN102945965A (en) * | 2012-11-27 | 2013-02-27 | 广东中科信泰新能源有限公司 | Preparing method of porous carbon embedding type lithium ion battery anode material |
| CN103303893A (en) * | 2013-06-04 | 2013-09-18 | 清华大学深圳研究生院 | Preparation method of lithium iron phosphate |
| CN103500832A (en) * | 2013-10-23 | 2014-01-08 | 山东大学 | Method of preparing nanoscale lithium iron phosphate / carbon composite anode material |
| CN103515578A (en) * | 2013-07-15 | 2014-01-15 | 江苏华东锂电技术研究院有限公司 | Preparation method of lithium ion battery anode material |
| CN103682344A (en) * | 2013-12-25 | 2014-03-26 | 天津斯特兰能源科技有限公司 | Method for synthetizing lithium iron phosphate material by utilizing sol-gel method |
| CN107188149A (en) * | 2017-07-31 | 2017-09-22 | 蒋央芳 | A kind of technique of LITHIUM BATTERY high-purity nm ferric phosphate |
| CN107732173A (en) * | 2017-09-25 | 2018-02-23 | 江苏奔拓电气科技有限公司 | A kind of preparation method of anode material for lithium-ion batteries |
| CN115148483A (en) * | 2022-07-28 | 2022-10-04 | 中国科学院生态环境研究中心 | Preparation of LiFe by using waste lithium iron phosphate battery 5 O 8 Method for producing magnetic material |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102491426A (en) * | 2011-12-09 | 2012-06-13 | 东莞市迈科科技有限公司 | Preparation method for lithium battery anode material LiNi0.5Mn1.5O4 |
| CN102491426B (en) * | 2011-12-09 | 2013-11-13 | 东莞市迈科科技有限公司 | Preparation method for lithium battery anode material LiNi0.5Mn1.5O4 |
| CN102496714A (en) * | 2011-12-27 | 2012-06-13 | 天津力神电池股份有限公司 | Anode active substance, production method thereof, and lithium ion battery employing anode active substance |
| CN102945965A (en) * | 2012-11-27 | 2013-02-27 | 广东中科信泰新能源有限公司 | Preparing method of porous carbon embedding type lithium ion battery anode material |
| CN103303893A (en) * | 2013-06-04 | 2013-09-18 | 清华大学深圳研究生院 | Preparation method of lithium iron phosphate |
| CN103303893B (en) * | 2013-06-04 | 2014-12-10 | 清华大学深圳研究生院 | Preparation method of lithium iron phosphate |
| CN103515578A (en) * | 2013-07-15 | 2014-01-15 | 江苏华东锂电技术研究院有限公司 | Preparation method of lithium ion battery anode material |
| CN103500832A (en) * | 2013-10-23 | 2014-01-08 | 山东大学 | Method of preparing nanoscale lithium iron phosphate / carbon composite anode material |
| CN103500832B (en) * | 2013-10-23 | 2017-05-24 | 山东大学 | Method of preparing nanoscale lithium iron phosphate / carbon composite anode material |
| CN103682344A (en) * | 2013-12-25 | 2014-03-26 | 天津斯特兰能源科技有限公司 | Method for synthetizing lithium iron phosphate material by utilizing sol-gel method |
| CN107188149A (en) * | 2017-07-31 | 2017-09-22 | 蒋央芳 | A kind of technique of LITHIUM BATTERY high-purity nm ferric phosphate |
| CN107732173A (en) * | 2017-09-25 | 2018-02-23 | 江苏奔拓电气科技有限公司 | A kind of preparation method of anode material for lithium-ion batteries |
| CN115148483A (en) * | 2022-07-28 | 2022-10-04 | 中国科学院生态环境研究中心 | Preparation of LiFe by using waste lithium iron phosphate battery 5 O 8 Method for producing magnetic material |
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Application publication date: 20110615 |