CN101508431A - Process for producing homodisperse spherical iron lithium phosphate - Google Patents
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- CN101508431A CN101508431A CNA2009100808559A CN200910080855A CN101508431A CN 101508431 A CN101508431 A CN 101508431A CN A2009100808559 A CNA2009100808559 A CN A2009100808559A CN 200910080855 A CN200910080855 A CN 200910080855A CN 101508431 A CN101508431 A CN 101508431A
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Abstract
The invention relates to a method for preparing uniformly dispersed spherical lithium iron phosphate-an anode material for a lithium ion battery, and belongs to the field of green energy materials. The method comprises the following steps: firstly, preparing a spherical iron phosphate precursor through liquid-phase homogeneous precipitation; secondly, performing predecomposition on the spherical iron phosphate precursor at a temperature of between 350 and 450 DEG C for 2 to 8 hours under the protection of inert gas; and thirdly, performing reaction at the temperature of between 550 and 800 DEG C for 2 to 24 hours to obtain the uniformly dispersed spherical lithium iron phosphate. The particle diameter of the product is between 100 and 200 nanometers, the tap density is between 1.6 and 2.0 g/cm<3>, and the specific capacity of initial discharge at the room temperature reaches 140 to 160 mAh/g. The method utilizes a liquid-phase spheroidization process to prepare the uniformly dispersed spherical lithium iron phosphate, has simple process, and is easy to realize industrialized production.
Description
Technical field
The invention belongs to green energy resource material field.Be particularly related to a kind of high-density spherical ferric lithium phosphate preparation method as anode material for lithium-ion batteries.
Background technology
Lithium ion battery is a kind of green high-capacity battery, advantage such as have that voltage height, energy density are big, good cycle, operating temperature range are wide, be widely used in the equipment such as notebook computer, mobile telephone, electronic instrument, portable power tool good prospects for application being arranged also in power truck and hybrid vehicle at present.Lithium ion battery under the situation expensive day by day in fossil energy, that environmental pollution is on the rise, has important researching value and good application future as a kind of green high-capacity battery.
Positive electrode material is the important component part of lithium ion battery, and positive electrode material commonly used has LiCoO
2, LiNiO
2, LiMn
2O
4, LiFePO
4LiCoO
2Be the positive electrode material of unique large-scale commercial, over-all properties is better, but the shortcoming that its existence costs an arm and a leg, toxicity is bigger.The LiMn of spinel structure
2O
4Cost is low, and security is good, but cycle performance is relatively poor.Iron lithium phosphate (the LiFePO of olivine structural
4) positive electrode material become the domestic and international research focus.
Relative and the positive electrode material LiCoO of the lithium iron phosphate positive material of olivine structural
2, LiMn
2O
4Advantage be: with low cost; Charge and discharge platform is stable; Good cycle; Stability Analysis of Structures, high-temperature behavior and safety performance are good; Nontoxic, environmental friendliness.But LiFePO
4Break two significant disadvantages, the one, specific conductivity is low, causes high-rate charge-discharge capability poor; The 2nd, tap density is low, thereby its volume and capacity ratio is also little.These two significant disadvantages have influenced the application of this material.
In order to solve this problem of iron lithium phosphate specific conductivity, the innovative approach that people take mainly is that iron lithium phosphate is carried out the carbon coating and doping small amount of impurities ion in the iron lithium phosphate lattice.Adopt new preparation technology, as sol-gel method, micro emulsion method, the particle of synthesis nano iron lithium phosphate can shorten the diffusion length of lithium ion, improves the lithium ion conductivity of material.By above method, the specific conductivity of iron lithium phosphate has obtained tangible improvement at present.
Yet solve the defective of iron lithium phosphate on tap density and then need more effort.Commercial cobalt acid lithium tap density generally can reach 2.2-2.6g/cm
3, and the tap density of iron lithium phosphate is generally 1.0-1.25g/cm
3, gap is obvious.Low tap density makes the volume and capacity ratio of iron lithium phosphate be starkly lower than cobalt acid lithium, does not have advantage in actual applications.
Studies show that from microscopic appearance, characteristic such as the pattern by improving powder granule and particle diameter can change the tap density of material.According to the literature, the regular spherical particle has higher tap density with respect to irregular particle.As in the patent of invention " preparation method of high-density spherical ferric lithium phosphate and iron manganese phosphate for lithium " of application number 200510002012.9, with source of iron, phosphorus source, complexing agent mixed aqueous solution and concentration is the ammonia soln reaction synthesizing spherical ferrous ammonium phosphate presoma of 2-10 mol, dry back high-temperature heat treatment obtains spherical LiFePO 4, the product particle diameter is 7-12 μ m, and tap density reaches 2.0-2.2g/cm
3, first discharge specific capacity reaches 145-160mAh/g under the room temperature.In the patent of invention " a kind of method for preparing solid phase of high-density spherical-like ferric phosphate lithium " of application number 200710028996.7, raw material is mixed and carries out wet ball-milling with the nucleus growth agent (nano-silver powder, copper nanoparticle etc.) of doping metals and 0.1-10wt.%, and dry back high-temperature heat treatment obtains LiFePO
4, the product tap density reaches 1.55-1.75g/cm
3, specific discharge capacity reaches 125-145mAh/g.In the patent of invention " preparation method of high-density spherical ferric lithium phosphate as anode material of lithium-ion battery " of application number 200410103485.3, be input to source of iron, phosphorus source, alkali aqueous solution in the reactor of band stirring respectively continuously with pump, flow and the pH value and the temperature etc. of the control source of iron and the phosphorus source aqueous solution, make the ball shape ferric phosphate presoma earlier, high-temperature heat treatment obtains LiFePO again
4, the product particle diameter is 7-12 μ m, tap density reaches 2.0-2.2g/cm
3, first discharge specific capacity reaches 140-155mAh/g under the room temperature.
Yet it is complicated that the preparation method of the spherical LiFePO 4 of having reported at present shows on preparation technology slightly, need control the flow of reaction solution or add precipitation agent (complexing agent) etc. as the liquid phase production method, and technology controlling and process is had relatively high expectations.Solid phase method prepares spherical LiFePO 4 generally need add the nucleus growth agent, and the chemical property of product is poor slightly.
Summary of the invention
The purpose of this invention is to provide the preparation method of a kind of technology homodisperse spherical iron lithium phosphate that is used as anode material for lithium-ion batteries simple, with low cost, prepared ball shape ferric phosphate lithium material has higher tap density and better electrochemical performance.
The LiFePO 4 material chemical constitution of the present invention's preparation is LiFe
aM
bPO
4, wherein M is selected from one or more of Mg, Al, Ti, V, Cr, Mn, Co, Ni, Zn, and 0.7≤a≤1,0≤b≤0.3, and this method is carried out according to following steps:
(1) configuration concentration is the source of iron aqueous solution of 0.01-3mol/l, and concentration is the aqueous metal salt of 0.01-3mol/l, and concentration is the phosphorus source aqueous solution of 0.01-3mol/l;
(2) the source of iron aqueous solution, aqueous metal salt and the phosphorus source aqueous solution are mixed in reaction vessel, obtain clarifying reaction solution, conditioned reaction liquid pH value is 1.0-5.5, and reaction solution is continued to stir one hour;
(3) reaction vessel is airtight, place 35-90 ℃ thermostat container, be incubated 0.5-48 hours and obtain precipitation, with precipitate and separate, washing, drying, obtain homodisperse spherical Fe
aM
bPO
4
(4) with the phosphoric acid salt that makes and lithium source, carbon source uniform mixing, under protection of inert gas, 350-450 ℃ of predecomposition 2-8 hours 550-800 ℃ of reactions 2-24 hours, obtains homodisperse spherical LiFe then
aM
bPO
4
This method also can be carried out according to following steps:
(1) configuration concentration is the source of iron aqueous solution of 0.01-3mol/l, and concentration is the aqueous metal salt of 0.01-3mol/l, and concentration is the phosphorus source aqueous solution of 0.01-3mol/l;
(2) dispose a kind of buffered soln;
(3) the source of iron aqueous solution, aqueous metal salt, the phosphorus source aqueous solution and buffering solution are mixed in reaction vessel, obtain clarifying reaction solution, conditioned reaction liquid pH value is 1.0-5.5, and reaction solution is continued to stir one hour;
(4) reaction vessel is airtight, place 35-90 ℃ thermostat container, be incubated 0.5-48 hours and obtain precipitation, with precipitate and separate, washing, drying, obtain homodisperse spherical Fe
aM
bPO
4
(5) with the phosphoric acid salt that makes and lithium source, carbon source uniform mixing.Under protection of inert gas, 350-450 ℃ of predecomposition 2-8 hours 550-800 ℃ of reactions 2-24 hours, obtains homodisperse spherical LiFe then
aM
bPO
4
Described metal-salt is selected from one or more of muriate, vitriol, nitrate, perchlorate of this metal.
Described phosphorus source is selected from H
3PO
4, NH
4H
2PO
4, (NH
4)
2HPO
4, Na
3PO
4, Na
2H
2PO
4, Na
2HPO
4, K
3PO
4, KH
2PO
4, K
2HPO
4One or more.
Described lithium source is selected from one or more in lithium chloride, Lithium Sulphate, lithium nitrate, Quilonum Retard, lithium hydroxide, the Lithium Acetate.
Described rare gas element is selected from one or more of argon gas, hydrogen, nitrogen.
Described buffered soln is selected from one or more of phosphate buffered saline buffer, acetate buffer, Padil-hydrochloric acid mixed solution, Mono Chloro Acetic Acid-sodium hydroxide mixed solution, formic acid-sodium hydroxide mixed solution.
The present invention can add tensio-active agent or complexing agent or add tensio-active agent and complexing agent simultaneously in the described reaction solution of step (1); Tensio-active agent is selected from one or more of polyvinylpyrrolidone, polyvinyl alcohol, polyoxyethylene glycol, cetyl trimethylammonium bromide (CTAB), Triton, this dish, tween; Complexing agent is selected from one or more of citric acid, tartrate, EDTA.
The invention has the beneficial effects as follows:
1. utilize the liquid phase method preparation all to disperse the tertiary iron phosphate presoma, low cost of raw materials, technology controlling and process is simple, and need not complicated conversion unit;
2. do not use complexing agent or precipitation agent etc., avoided the introducing of foreign ion such as ammonium ion;
3. prepared spherical equal dispersive iron lithium phosphate, tap density is higher, and chemical property is better.
Description of drawings
Fig. 1 is a sem photograph of pressing the iron phosphate powder of embodiment 1 preparation;
Fig. 2 is an X-ray powder diffraction collection of illustrative plates of pressing the iron phosphate powder of embodiment 1 preparation;
Fig. 3 is a first charge-discharge curve of pressing the iron phosphate powder of embodiment 1 preparation.
Embodiment
State the present invention below by specific embodiment is next auspicious, but be not limited thereto.
Embodiment 1
Take by weighing the 4.0544g iron trichloride, add 300ml distilled water, obtain source of iron solution.Measure 2.153ml phosphoric acid, take by weighing the 2.1061g SODIUM PHOSPHATE, MONOBASIC, add 300ml distilled water, obtain 0.15 mol phosphorus source solution.Regulate the pH value to 1.5 of phosphorus source solution with hydrochloric acid.Source of iron solution is slowly added in the solution of phosphorus source, and constantly stir, obtain reaction solution, continue to stir one hour.Reaction solution is placed encloses container, place 35 ℃ thermostat container then, be incubated after 48 hours and take out, obtain precipitation.With precipitate and separate, washing, drying obtain the homodisperse spherical tertiary iron phosphate.Take by weighing the 1.8682g tertiary iron phosphate, 0.7389g Quilonum Retard, and 2% acetylene black mix back ball milling 2 hours in ball mill.Mixed powder is transferred in the quartz boat, placed tube furnace then, under argon shield, 350 ℃ of predecomposition 8 hours 550 ℃ of reactions 12 hours, obtains homodisperse spherical iron lithium phosphate then.Product cut size 100-200nm, tap density 1.8g/cm
3, first discharge specific capacity reaches 149.2mAh/g under the room temperature.
The material pattern is seen accompanying drawing 1;
Material X-ray powder diffraction collection of illustrative plates is seen accompanying drawing 2;
Material first charge-discharge curve is seen accompanying drawing 3.
Take by weighing the 27.0290g iron trichloride, add 200ml distilled water, obtain source of iron solution.Measure 14.35ml phosphoric acid, take by weighing the 14.0409g SODIUM PHOSPHATE, MONOBASIC, add 200ml distilled water, obtain 1.5 mol phosphorus source solution.Regulate the pH value to 1.8 of phosphorus source solution with hydrochloric acid.Source of iron solution is slowly added in the solution of phosphorus source, and constantly stir, obtain reaction solution, continue to stir one hour.Reaction solution is placed encloses container, place 90 ℃ thermostat container then, be incubated after 30 minutes and take out, obtain precipitation.With precipitate and separate, washing, drying, obtain the homodisperse spherical tertiary iron phosphate.Take by weighing the 9.3410g tertiary iron phosphate, 2.0980g lithium hydroxide (LiOHH
2O), 0.8764g glucose, 1.4245g magnesium nitrate (Mg (NO
3)
2H
2O), mix back ball milling 5 hours in ball mill.Mixed powder is transferred in the quartz boat, placed tube furnace then, under argon shield, 450 ℃ of predecomposition 2 hours 800 ℃ of reactions 2 hours, obtains homodisperse spherical trimagnesium phosphate iron lithium (LiFe then
0.9Mg
0.1PO
4).Product cut size 100-200nm, tap density 1.7g/cm
3, first discharge specific capacity reaches 157.6mAh/g under the room temperature.
Claims (10)
1. the preparation method of a homodisperse spherical iron lithium phosphate, its chemical constitution is LiFe
aM
bPO
4, wherein M is selected from one or more of Mg, Al, Ti, V, Cr, Mn, Co, Ni, Zn, and 0.7≤a≤1,0≤b≤0.3, it is characterized in that may further comprise the steps:
(1) configuration concentration is the source of iron aqueous solution of 0.01-3mol/l, and concentration is the aqueous metal salt of 0.01-3mol/l, and concentration is the phosphorus source aqueous solution of 0.01-3mol/l;
(2) the source of iron aqueous solution, aqueous metal salt and the phosphorus source aqueous solution are mixed in reaction vessel, obtain clarifying reaction solution, conditioned reaction liquid pH value is 1.0-5.5, and reaction solution is continued to stir one hour;
(3) reaction vessel is airtight, place 35-90 ℃ thermostat container, be incubated 0.5-48 hours and obtain precipitation, with precipitate and separate, washing, drying, obtain homodisperse spherical Fe
aM
bPO
4
(4) with the phosphoric acid salt that makes and lithium source, carbon source uniform mixing, under protection of inert gas, 350-450 ℃ of predecomposition 2-8 hours 550-800 ℃ of reactions 2-24 hours, obtains homodisperse spherical LiFe then
aM
bPO
4
2. by the preparation method of the described homodisperse spherical iron lithium phosphate of claim 1, it is characterized in that: the preparation method may further comprise the steps:
(1) configuration concentration is the source of iron aqueous solution of 0.01-3mol/l, and concentration is the aqueous metal salt of 0.01-3mol/l, and concentration is the phosphorus source aqueous solution of 0.01-3mol/l;
(2) dispose a kind of buffered soln;
(3) the source of iron aqueous solution, aqueous metal salt, the phosphorus source aqueous solution and buffering solution are mixed in reaction vessel, obtain clarifying reaction solution, conditioned reaction liquid pH value is 1.0-5.5, and reaction solution is continued to stir one hour;
(4) reaction vessel is airtight, place 35-90 ℃ thermostat container, be incubated 0.5-48 hours and obtain precipitation, with precipitate and separate, washing, drying, obtain homodisperse spherical Fe
aM
bPO
4
(5) with the phosphoric acid salt that makes and lithium source, carbon source uniform mixing; Under protection of inert gas, 350-450 ℃ of predecomposition 2-8 hours 550-800 ℃ of reactions 2-24 hours, obtains homodisperse spherical LiFe then
aM
bPO
4
3. by the preparation method of the described homodisperse spherical iron lithium phosphate of claim 1, it is characterized in that: described metal-salt is selected from one or more of muriate, vitriol, nitrate, perchlorate of this metal.
4. by the preparation method of the described homodisperse spherical iron lithium phosphate of claim 1, it is characterized in that: described phosphorus source is selected from H
3PO
4, NH
4H
2PO
4, (NH
4)
2HPO
4, Na
3PO
4, Na
2H
2PO
4, Na
2HPO
4, K
3PO
4, KH
2PO
4, K
2HPO
4One or more.
5. by the preparation method of the described homodisperse spherical iron lithium phosphate of claim 1, it is characterized in that: described lithium source is selected from one or more in lithium chloride, Lithium Sulphate, lithium nitrate, Quilonum Retard, lithium hydroxide, the Lithium Acetate.
6. by the preparation method of the described homodisperse spherical iron lithium phosphate of claim 1, it is characterized in that: in the described reaction solution of step (1), add tensio-active agent or complexing agent or add tensio-active agent and complexing agent simultaneously.
7. by the preparation method of the described homodisperse spherical iron lithium phosphate of claim 6, it is characterized in that: described tensio-active agent is selected from one or more of polyvinylpyrrolidone, polyvinyl alcohol, polyoxyethylene glycol, cetyl trimethylammonium bromide (CTAB), Triton, this dish, tween.
8. by the preparation method of the described homodisperse spherical iron lithium phosphate of claim 6, it is characterized in that: described complexing agent is selected from one or more of citric acid, tartrate, EDTA.
9. want the preparation method of 1 described homodisperse spherical iron lithium phosphate by right, it is characterized in that: described rare gas element is selected from one or more of argon gas, hydrogen, nitrogen.
10. by the preparation method of the described homodisperse spherical iron lithium phosphate of claim 2, it is characterized in that: described buffered soln is selected from one or more of phosphate buffered saline buffer, acetate buffer, Padil-hydrochloric acid mixed solution, Mono Chloro Acetic Acid-sodium hydroxide mixed solution, formic acid-sodium hydroxide mixed solution.
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| CN102255078A (en) * | 2011-05-27 | 2011-11-23 | 丁建民 | Coordinated method for preparing nanometer spherical iron phosphate and then using carbon fusion method to prepare nanometer spherical lithium iron phosphate |
| CN102593452A (en) * | 2012-03-22 | 2012-07-18 | 华南师范大学 | Method for preparing carbon-coated lithium iron phosphate material |
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| CN107324306A (en) * | 2017-07-18 | 2017-11-07 | 江西悦安超细金属有限公司 | A kind of nano-grade lithium iron phosphate and preparation method thereof |
| CN108539132A (en) * | 2018-01-26 | 2018-09-14 | 澳洋集团有限公司 | A kind of preparation method of zinc oxide-lithium iron phosphate composite anode material |
| CN111217346A (en) * | 2019-11-22 | 2020-06-02 | 贵州唯特高新能源科技有限公司 | Preparation method of high-performance ferrous phosphate |
| CN111816851A (en) * | 2020-06-22 | 2020-10-23 | 南昌大学 | Hierarchical porous LiMnxFe1-xPO4Template-free hydrothermal preparation method of/C composite microsphere cathode material |
| WO2023060743A1 (en) * | 2021-10-11 | 2023-04-20 | 中国科学院过程工程研究所 | Lithium ion battery positive electrode material, and preparation method therefor and use thereof |
| WO2023116019A1 (en) * | 2021-12-22 | 2023-06-29 | 广东邦普循环科技有限公司 | Lithium iron phosphate material and preparation method therefor |
| GB2616238A (en) * | 2021-12-22 | 2023-08-30 | Guangdong Brunp Recycling Technology Co Ltd | Lithium iron phosphate material and preparation method therefor |
| CN115321506A (en) * | 2022-07-28 | 2022-11-11 | 安徽格派新能源有限公司 | Preparation method of high-compaction modified lithium manganese iron phosphate cathode material |
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