CN101593831A - Process for preparing sol-gel based on the lithium iron phosphate cathode material of ferric phosphate - Google Patents
Process for preparing sol-gel based on the lithium iron phosphate cathode material of ferric phosphate Download PDFInfo
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- CN101593831A CN101593831A CNA2009100694721A CN200910069472A CN101593831A CN 101593831 A CN101593831 A CN 101593831A CN A2009100694721 A CNA2009100694721 A CN A2009100694721A CN 200910069472 A CN200910069472 A CN 200910069472A CN 101593831 A CN101593831 A CN 101593831A
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- lithium
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- ferric phosphate
- lithium iron
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Abstract
The present invention relates to process for preparing sol-gel based on the lithium iron phosphate cathode material of ferric phosphate; earlier ferric phosphate and Li source compound are mixed in proportion; add organic complexing agent and carbon-source cpd then; be dissolved in water and constant temperature stirring formation colloidal sol; heat drying is until forming gel again; after mixing abundant ball milling; first in uniform temperature pre-burning a period of time under inert gas shielding in tube furnace; under the last inert gas shielding; in uniform temperature calcining at constant temperature certain hour, can make lithium iron phosphate cathode material.The present invention is raw material with the ferric phosphate, and the source is enriched and cheaply is easy to get, and greatly reduces cost; And the present invention adopts sol-gel process to make reactant realize that molecular level mixes, and cuts down the consumption of energy thereby greatly reduce reaction temperature, prepares the lithium iron phosphate cathode material of function admirable.
Description
[technical field]
The present invention relates to the lithium-ions battery field, particularly based on the process for preparing sol-gel of the lithium iron phosphate cathode material of ferric phosphate.
[background technology]
Lithium ion battery is the novel green high-power rechargeable battery that occurs early 1990s, has become the emphasis that competitively research and develop countries in the world at present.Common anode material for lithium-ion batteries has LiCoO
2, LiNiO
2, LiMn
2O
4Deng, but LiCoO
2Toxic, Capacity Ratio is lower, cost of material height, and the poor performance of overcharging; LiNiO
2Be difficult to preparation, cost of material is also than higher, and preparation temperature is very high, and energy consumption is big; LiMn
2O
4John-Teller effect, structural instability take place in charge and discharge process easily.So develop a kind of capacity height, cheap, preparation is simple, Stability Analysis of Structures, eco-friendly positive electrode become research focus.
LiFePO
4It is a kind of novel anode material for lithium-ion batteries.Its theoretical capacity height has good charge and discharge platform, excellent cycle performance, and cheap, advantages of environment protection is considered to the most rising anode material for lithium-ion batteries.Be widely used in industrial production aspects such as mine lamp at present, and progressively be applied to high-tech areas such as notebook computer, battery of mobile phone, and to be expected to be applied in the lithium ion battery be on the electric automobile of power that its future is immeasurable.
The preparation method of ferrousphosphate lithium material mainly contains high temperature solid-phase sintering method, carbothermic method, coprecipitation, hydro thermal method or the like at present.Yet all there are some intrinsic shortcomings in these methods, and as the synthesis temperature height, synthesis cycle is long, controlled condition is harsh, cost is high and the large current discharging capability difference of synthetic material etc.These shortcomings have all limited the extensive industrialization of LiFePO 4.
[summary of the invention]
The objective of the invention is in order to overcome the deficiencies in the prior art, and process for preparing sol-gel based on the lithium iron phosphate cathode material of ferric phosphate is provided, the raw material sources that this process for preparing sol-gel uses are abundant, synthesis temperature is low, synthesis cycle is short, condition control is easy, synthetic method simply, production cost is very low.
The present invention is that to address the above problem the scheme that is adopted be the process for preparing sol-gel of design based on the lithium iron phosphate cathode material of ferric phosphate.It is characterized in that ferric phosphate, Li source compound and organic complex, ferric phosphate in molar ratio: Li source compound: organic complex is 1: 1: 1～1: 1: 10 a mixed, and then the carbon-source cpd of adding 0-20wt%, prepare by sol-gel process.
The process for preparing sol-gel of described lithium iron phosphate cathode material based on ferric phosphate, it is characterized in that preparation process is: with ferric phosphate, Li source compound and organic complexing agent in proportion adding distil water make it dissolving and form colloidal sol, hour make gel in 30-90 ℃ of following heated at constant temperature, stirring, evaporation 0.5-5 then, final drying gets xerogel; To put into tube furnace behind the xerogel ball milling, under inert gas shielding in 300-450 ℃ of constant temperature pre-burning 4-12 hour; Under inert gas shielding, heat up then with the rate of heat addition of 10 ℃/min, rise to 500-800 ℃ after calcining at constant temperature 4-24 hour, the rate of temperature fall with 10 ℃/min is cooled to room temperature at last, can obtain lithium ferrous phosphate as anode material of lithium ion battery.
Of the present invention have a following advantage:
1, the required primary raw material of material preparation source is rich and easy to get, cheap, and cost is lower.
2, raw material is source of iron with the ferric phosphate, compares with the divalence source of iron, has reduced the anionic kind of impurity, the high material of easier preparation purity.
3, the present invention adopts sol-gal process, and operation is simple, has reduced preparation temperature, thereby has reduced technological parameter, has further reduced energy consumption and cost.
4, the present invention adopts sol-gal process, makes raw material be molecular level and mixes, and mixes extremely evenly, helps the material of processability stable homogeneous.
5, Zhi Bei material has the discharge platform about 3.4V stably, its discharge capacity height, and its first discharge specific capacity reaches 165.3mAh/g during the 0.1C discharge, is 136.3mAh/g during 1C; Its cycle performance is good, and when 0.1C and 1C discharge, 50 all after date capacity that circulate remain on 154.2mAh/g and 133.6mAh/g respectively.
6, Zhi Bei material structure is stable, and not containing Co, Ni etc. has the element of bigger pollution to environment, thereby is environmentally friendly material, is well suited for suitability for industrialized production.
[description of drawings]
Fig. 1 is the XRD figure of the prepared lithium iron phosphate cathode material of embodiment 1;
Fig. 2 is the prepared first discharge capacity curve of simulation lithium ion battery when 0.1C and 1C of embodiment 2;
Fig. 3 is the prepared cycle performance curve of simulation lithium ion battery when 0.1C and 1C of embodiment 3.
Be described in detail with reference to accompanying drawing below in conjunction with embodiments of the invention.
[embodiment]
For the technical solution problem; the process for preparing sol-gel of a kind of lithium ferrous phosphate as anode material of lithium ion battery based on ferric phosphate provided by the invention; its concrete implementation step is: with ferric phosphate; Li source compound is a raw material; it is mixed in proportion; adding carbon source and organic complexing agent is dissolved in the distilled water; and stir 0.5-5 hour until forming colloidal sol in 30-90 ℃ of heated at constant temperature; this colloidal sol drying is obtained xerogel; put into tube furnace after mixing ball milling; under inert gas shielding in 300-450 ℃ of constant temperature pre-burning 4-12 hour, at last under inert gas shielding in 500-800 ℃ of calcining at constant temperature 4-24 hour.
A kind of in the optional lithium hydroxide in the used lithium of the present invention source, lithia, lithium nitrate, lithium carbonate, lithium oxalate, lithium acetate, lithium sulfate, lithium chloride, lithium fluoride or the lithium citrate etc.;
The used source of iron of the present invention is a ferric phosphate;
A kind of in the optional malonic acid of the used organic complexing agent of the present invention, malonic acid ammonium, citric acid, ammonium citrate, ascorbic acid, ascorbic acid ammonium, malic acid, malic acid ammonium, gluconic acid, ammonium gluconate, oxalic acid, ammonium oxalate, lactic acid or the ammonium lactate etc.
A kind of in the optional sucrose of the used carbon-source cpd of the present invention, glucose, maltose, fructose, lactose, PEG or the acetylene black etc.
Described heating whipping temp can be 50-70 ℃, and the time that flashes to gel is 3-5 hour.
Described calcined temperature can be 350-400 ℃, and the time is 4-8 hour.
Described calcining heat can be 550-700 ℃, and the time is 8-12 hour.
The used inert gas of the present invention can be Ar or N
2
Embodiment one
Take by weighing the 1.1213g ferric phosphate, 0.7943g oxalic acid, 0.4344g lithium nitrate and 0.2248g sucrose, the adding distil water dissolving is stirred 2 hours formation gels down at 65 ℃, puts into the baking oven drying then and obtains xerogel; Xerogel is ground the back compressing tablet, put into tube furnace under inert gas shielding in 300 ℃ of pre-burnings 6 hours, obtain lithium iron phosphate precursor.
Compressing tablet again after presoma ground, put into tube furnace under inert gas shielding in 600 ℃ of calcinings 8 hours, obtain lithium iron phosphate cathode material.
Fig. 1 is the XRD figure of gained material, and employing Rigaku D/Max III type X-ray diffractometer (Cu target ka ray, wavelength X=0.15418nm).The reference standard card as can be seen, synthetic material is olivine-type (space group Pnma), does not find the diffraction maximum of carbon in the spectrogram, the carbon in the illustrative material exists with amorphous forms.
The gained material is made electrode as follows:
Take by weighing material, conductive carbon and the polytetrafluoroethylene of embodiment one gained with 85: 10: 5 mass ratioes, mix and grind, making diameter then is the circular pole piece of 8mm, drying obtained positive plate in 24 hours in 100 ℃ of drying boxes, with the pure metal lithium sheet is negative pole, to be dissolved in the 1.0mol/L LiPF in EC+DMC (volume ratio is 1: the 1) mixed solvent
6Be electrolyte, polypropylene microporous film is a diaphragm material, forms the simulation lithium ion battery.
Embodiment two
Take by weighing 1.1213g ferric phosphate, 0.2216g lithium carbonate, 1.3238g citric acid, the adding distil water dissolving is stirred evaporation down at 90 ℃ and was formed gel in 1 hour, puts into the baking oven drying then and obtains xerogel; Xerogel is ground the back compressing tablet, put into tube furnace under inert gas shielding in 400 ℃ of pre-burnings 3 hours, obtain lithium iron phosphate precursor.
Compressing tablet again after presoma ground, put into tube furnace under inert gas shielding in 650 ℃ of calcinings 6 hours, obtain lithium iron phosphate cathode material.
The gained material is made electrode as follows:
Take by weighing material, conductive carbon and the polytetrafluoroethylene of embodiment two gained with 85: 10: 5 mass ratioes, mix and grind, making diameter then is the circular pole piece of 8mm, drying obtained positive plate in 24 hours in 100 ℃ of drying boxes, with the pure metal lithium sheet is negative pole, to be dissolved in the 1.0mol/L LiPF in EC+DMC (volume ratio is 1: the 1) mixed solvent
6Be electrolyte, polypropylene microporous film is a diaphragm material, forms the simulation lithium ion battery.
Fig. 2 is the first discharge curve of gained material when 0.1C and 1C, and probe temperature is a room temperature.As can be seen from the figure: when discharging and recharging by voltage is 2.5-4.2V, and charge-discharge magnification is when 0.1C, and the material of measuring and monitoring the growth of standing timber has the discharge voltage plateau about 3.4V, and the first discharge specific capacity of material is 165.3mAh/g; When discharge-rate was elevated to 1C, the first discharge specific capacity of this material reached 136.3mAh/g.
Embodiment three
Take by weighing 1.1213g ferric phosphate, 0.2518g lithium hydroxide, 1.0568g ascorbic acid, the adding distil water dissolving is stirred evaporation down at 85 ℃ and was formed gel in 1.5 hours, puts into oven drying then and obtains xerogel; Xerogel is ground the back compressing tablet, put into tube furnace under inert gas shielding in 350 ℃ of pre-burnings 4 hours, obtain lithium iron phosphate precursor.
Compressing tablet again after presoma ground, put into tube furnace under inert gas shielding in 700 ℃ of calcinings 4 hours, obtain lithium iron phosphate cathode material.
The gained material is made electrode as follows:
Take by weighing material, conductive carbon and the polytetrafluoroethylene of embodiment three gained with 85: 10: 5 mass ratioes, mix and grind, making diameter then is the circular pole piece of 8mm, drying obtained positive plate in 24 hours in 100 ℃ of drying boxes, with the pure metal lithium sheet is negative pole, to be dissolved in the 1.0mol/L LiPF in EC+DMC (volume ratio is 1: the 1) mixed solvent
6Be electrolyte, polypropylene microporous film is a diaphragm material, forms the simulation lithium ion battery.
Fig. 3 is the cycle performance curve of gained material when 0.1C and 1C.As can be seen from the figure, the gained material is respectively when 0.1C and 1C multiplying power discharging, and 50 all after date specific discharge capacities that circulate are respectively 154.2 and 133.6mAh/g, and capability retention is respectively 93.28% and 98.02%.
Claims (9)
1. based on the process for preparing sol-gel of the lithium iron phosphate cathode material of ferric phosphate, it is characterized in that ferric phosphate, Li source compound and organic complex, ferric phosphate in molar ratio: Li source compound: organic complex is 1: 1: 1～1: 1: 10 a mixed, and then the carbon-source cpd of adding 0-20wt%, prepare by sol-gel process.
2. the process for preparing sol-gel of the lithium iron phosphate cathode material based on ferric phosphate according to claim 1 is characterized in that preparation process is:
With ferric phosphate, Li source compound and organic complexing agent in proportion adding distil water make it dissolving and form colloidal sol, hour make gel in 30-90 ℃ of following heated at constant temperature, stirring, evaporation 0.5-5 then, final drying gets xerogel; To put into tube furnace behind the xerogel ball milling, under inert gas shielding in 300-450 ℃ of constant temperature pre-burning 4-12 hour; Under inert gas shielding, heat up then with the rate of heat addition of 10 ℃/min, rise to 500-800 ℃ after calcining at constant temperature 4-24 hour, the rate of temperature fall with 10 ℃/min is cooled to room temperature at last, can obtain lithium ferrous phosphate as anode material of lithium ion battery.
3. the process for preparing sol-gel of the lithium iron phosphate cathode material based on ferric phosphate according to claim 1 and 2 is characterized in that Li source compound is a kind of in lithium hydroxide, lithia, lithium nitrate, lithium carbonate, lithium oxalate, lithium acetate, lithium sulfate, lithium chloride, lithium fluoride or the lithium citrate.
4. the process for preparing sol-gel of the lithium iron phosphate cathode material based on ferric phosphate according to claim 1 and 2 is characterized in that organic complexing agent is a kind of in malonic acid, malonic acid ammonium, citric acid, ammonium citrate, ascorbic acid, ascorbic acid ammonium, malic acid, malic acid ammonium, gluconic acid, ammonium gluconate, oxalic acid, ammonium oxalate, lactic acid or the ammonium lactate.
5. the process for preparing sol-gel of the lithium iron phosphate cathode material based on ferric phosphate according to claim 1 and 2 is characterized in that carbon-source cpd is a kind of in sucrose, glucose, maltose, fructose, lactose, PEG or the acetylene black.
6. the process for preparing sol-gel of the lithium iron phosphate cathode material based on ferric phosphate according to claim 2, it is characterized in that heating whipping temp is 50-70 ℃, the time that flashes to gel is 3-5 hour.
7. the process for preparing sol-gel of the lithium iron phosphate cathode material based on ferric phosphate according to claim 2 is characterized in that calcined temperature is 350-400 ℃, and the time is 4-8 hour.
8. the process for preparing sol-gel of the lithium iron phosphate cathode material based on ferric phosphate according to claim 2 is characterized in that calcining heat is 550-700 ℃, and the time is 8-12 hour.
9. the process for preparing sol-gel of the lithium iron phosphate cathode material based on ferric phosphate according to claim 2 is characterized in that described inert gas is Ar or N
2
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| CNA2009100694721A CN101593831A (en) | 2009-06-29 | 2009-06-29 | Process for preparing sol-gel based on the lithium iron phosphate cathode material of ferric phosphate |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633250A (en) * | 2012-03-29 | 2012-08-15 | 天津巴莫科技股份有限公司 | High-voltage anode material for lithium ion batteries and method for preparing high-voltage anode material |
| CN102115067B (en) * | 2009-12-31 | 2012-11-28 | 河南科隆集团有限公司 | Preparation method of spherical lithium iron phosphate with good conductive network |
| CN103219516A (en) * | 2013-04-07 | 2013-07-24 | 中国科学院新疆理化技术研究所 | Preparation method of phosphate potential boron-doped carbon-wrapped phosphoric acid iron-lithium material |
| EP2746220A3 (en) * | 2012-12-21 | 2014-07-30 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Particles with a large surface coated with an intercalation material, method for the production thereof and use of the particles in hybrid electrodes and high capacity double layer capacitors and quick batteries |
| WO2014161742A1 (en) * | 2013-04-04 | 2014-10-09 | Chemische Fabrik Budenheim Kg | Amorphized iron(iii) phosphate |
| CN113991070A (en) * | 2021-09-14 | 2022-01-28 | 陕西创普斯新能源科技有限公司 | Lithium iron phosphate composite material and preparation method and application 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 |
| WO2024159919A1 (en) * | 2023-01-31 | 2024-08-08 | 湖北亿纬动力有限公司 | Composite lithium iron phosphate positive electrode material, preparation method therefor and use thereof |
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2009
- 2009-06-29 CN CNA2009100694721A patent/CN101593831A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115067B (en) * | 2009-12-31 | 2012-11-28 | 河南科隆集团有限公司 | Preparation method of spherical lithium iron phosphate with good conductive network |
| CN102633250A (en) * | 2012-03-29 | 2012-08-15 | 天津巴莫科技股份有限公司 | High-voltage anode material for lithium ion batteries and method for preparing high-voltage anode material |
| EP2746220A3 (en) * | 2012-12-21 | 2014-07-30 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Particles with a large surface coated with an intercalation material, method for the production thereof and use of the particles in hybrid electrodes and high capacity double layer capacitors and quick batteries |
| WO2014161742A1 (en) * | 2013-04-04 | 2014-10-09 | Chemische Fabrik Budenheim Kg | Amorphized iron(iii) phosphate |
| CN103219516A (en) * | 2013-04-07 | 2013-07-24 | 中国科学院新疆理化技术研究所 | Preparation method of phosphate potential boron-doped carbon-wrapped phosphoric acid iron-lithium material |
| CN103219516B (en) * | 2013-04-07 | 2015-04-22 | 中国科学院新疆理化技术研究所 | Preparation method of phosphate potential boron-doped carbon-wrapped phosphoric acid iron-lithium material |
| CN113991070A (en) * | 2021-09-14 | 2022-01-28 | 陕西创普斯新能源科技有限公司 | Lithium iron phosphate composite material and preparation method and application 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 |
| US12098072B2 (en) | 2021-12-22 | 2024-09-24 | Guangdong Brunp Recycling Technology Co., Ltd. | Lithium iron phosphate material and preparation method therefor |
| WO2024159919A1 (en) * | 2023-01-31 | 2024-08-08 | 湖北亿纬动力有限公司 | Composite lithium iron phosphate positive electrode material, preparation method therefor and use thereof |
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Open date: 20091202 |