CN101759172A - Microwave sintering method for preparing high-performance iron phosphate lithium - Google Patents
Microwave sintering method for preparing high-performance iron phosphate lithium Download PDFInfo
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Abstract
The invention relates to a microwave sintering method for preparing high-performance iron phosphate lithium, which belongs to the new technical field of energy materials. The method comprises the following steps of: firstly, mixing ferrous sulfate, a phosphorus source and a complexing agent or further adding manganous sulfate proportionally to prepare the water solution of the mixture; then, reacting with an ammonia solution to synthesize the precursor of spherical ferrous ammonium phosphate or ferrous ammonium manganese phosphate, after washing and drying, uniformly mixing with lithium carbonate in the mol ratio of 1:1, and adding a right amount of carbon source; after drying, preforming by using a preforming machine under the pressure of 10-40 MPa, and embedding into a pot full of carbon used for absorbing microwaves and producing protection atmosphere; placing the pot into a microwave oven, and heating at the microwave power of 100-800 W for 1-20 min; after heating, naturally cooling the pot to room temperature to obtain the spherical iron phosphate lithium. The spherical iron phosphate lithium prepared by the method and used as an anode material of lithium ion battery has high stacking density and high volume specific capacity, and the average grain diameter thereof is 5-12 tm, the tap density can reach 2.0-2.2 g/cm<3>, and the first discharge specific capacity at room temperature can reach 140-160 mA/g.
Description
Technical field
The present invention relates to a kind of microwave sintering method for preparing high-performance iron phosphate lithium, it belongs to energy new material technology field.
Background technology
Lithium ion battery is the green high-capacity battery of a new generation, numerous advantages such as have that voltage height, energy density are big, good cycle, self-discharge are little, memory-less effect, operating temperature range are wide, be widely used in mobile telephone, notebook computer, UPS, video camera, various portable power tool, electronic instrument, weaponry etc., in electromobile, also have a good application prospect, be considered to be in 21st century national economy and the significant new high-tech product of people's lives.
Positive electrode material is the important component part of lithium ion battery.At present, the maximum positive electrode material of research is LiCoO
2, LiNiO
2, LiMn
2O
4LiCoO
2Be the positive electrode material of unique large-scale commercial, the research comparative maturity, high comprehensive performance, but it costs an arm and a leg, and capacity is lower, and toxicity is bigger, has certain safety issue, and expectation will be replaced by the type material of high-performance and low-cost.And LiNiO
2Cost is lower, and capacity is higher, but the preparation difficulty, and there are comparatively serious safety problem in the consistence of material property and poor reproducibility.Spinel LiMn
2O
4Cost is low, and security is good, but cycle performance especially high temperature cyclic performance is poor, certain dissolubility is arranged in electrolytic solution, storge quality is poor.The research and development novel anode material becomes current focus.
Iron lithium phosphate (the LiFePO of quadrature olivine structural
4) positive electrode material becomes new research focus both at home and abroad gradually.Preliminary study shows that this novel anode material has been concentrated LiCoO
2, LiNiO
2, LiMn
2O
4Advantage separately Deng material: do not contain noble element, raw material cheapness, resource are greatly abundant; Operating voltage moderate (3.4V): platform identity is good, and voltage pole is (can match in excellence or beauty with voltage stabilized source) steadily; Theoretical capacity big (170rMh/g); Stability Analysis of Structures, safety performance splendid (O and P make material be difficult to analyse oxygen and decompose with the strong covalent bond mortise); High-temperature behavior and cycle performance traitor: volume-diminished during charging, the volume effect when cooperating with carbon negative pole material is good; Good with most of electrolyte system consistencies, storge quality is good; Nontoxic, be real green material.
Yet there are two significant disadvantages in iron lithium phosphate, the one, and specific conductivity is low, causes high-rate charge-discharge capability poor, reality, specific storage is low; The 2nd, tap density is low, causes volume and capacity ratio low.These two shortcomings have hindered the practical application of this material.Current, people's research attention concentrates on and solves low this field of iron lithium phosphate specific conductivity, and has obtained major progress.The innovative approach of taking mainly contains:
(1) mixes conductive carbon material or conductive metal particle toward the iron lithium phosphate granule interior,, improve the electronic conductivity of material perhaps toward iron lithium phosphate particle surface coated with conductive carbon material.
(2) in the iron lithium phosphate lattice, mix the small amount of impurities metal ion,, Zr4 wide as Mg2+, Al3+, T), Nb "; replace the position of a part of Li ', thereby make the iron lithium phosphate proper semiconductor change n type or p N-type semiconductorN into, significantly improved the electronic conductivity of material.
(3) in iron lithium phosphate, mix Mn
2+Deng impurity element, replace a part of Fe
2+The position, increase the unit cell parameters of iron lithium phosphate, improve the lithium ion conductivity of material, synthetic iron manganese phosphate for lithium (LiFex-,, MmPO4,0＜x≤0.4).
(4) adopt novel procesies such as sol-gel method, liquid phase synthesizing method, reduce the size of iron lithium phosphate crystal grain, even the synthesis of nano iron lithium phosphate, Li shortened as far as possible
+Diffusion length, improved the lithium ion conductivity and the material use efficiency of material on apparent.
Yet the shortcoming that the iron lithium phosphate tap density is low is subjected to people's ignorance and avoidance always, is not resolved as yet, has hindered the practical application of material.The theoretical density of cobalt acid lithium is 5.1g/cm
3, the tap density of commodity cobalt acid lithium is generally 2.0-2.4g/cm
3And the theoretical density of iron lithium phosphate only is 3.6g/cm
3, itself is just much lower than cobalt acid lithium.For improving electroconductibility, people mix conductive carbon material, have significantly reduced the tap density of material again, make the tap density of general carbon dope iron lithium phosphate have only 1.0g/cm
3So low tap density makes that the volume and capacity ratio of iron lithium phosphate is more much lower than the sour lithium of cobalt, and the battery volume of making will be very huge, not only have no advantage and can say, and be difficult to be applied to reality.Therefore, the tap density of raising iron lithium phosphate and volume and capacity ratio have the decision meaning to the practicability of iron lithium phosphate.
The tap density of powder body material and the pattern of powder granule, particle diameter and distribution thereof are closely related.Lithium iron phosphate positive material all is made up of random sheet or granular particle when having reported both at home and abroad at present, and tap density is low.The LiFePO 4 powder material of being made up of the spheroidal particle of rule will have higher tap density.Moreover, spherical product also has excellent flowability, dispersiveness and processability, very helps making the coating of positive electrode material slurry and electrode slice, improves the electrode slice quality.In addition, with respect to random particle, the spheroidal particle surface ratio of rule is easier to coat complete, even, firm decorative layer, so spherical LiFePO 4 more is hopeful further to improve over-all properties by finishing.
In application number is 200410103485.3 patent of invention " preparation method of high-density spherical ferric lithium phosphate as anode material of lithium-ion battery "; a kind of preparation method of high-density spherical ferric lithium phosphate is disclosed; this method is earlier with the trivalent iron salt aqueous solution, the phosphorus source aqueous solution, alkali aqueous solution reaction synthesizing spherical or class ball shape ferric phosphate presoma; the dry back of washing and lithium source, carbon source, doping metals compound uniform mixing; under inertia or protection of reducing atmosphere, obtained iron lithium phosphate in high-temperature heat treatment 8-48 hour through 600-900 ℃.The iron lithium phosphate median size that this method is prepared is 7-12um, and tap density can reach 2.0-2.2g/cm
3, first discharge specific capacity can reach 140-155mAh/g under the room temperature.In application number is 200510000167.9 patent of invention " a kind of preparation method of high-density spherical ferric lithium phosphate ", a kind of preparation method of high-density spherical ferric lithium phosphate is disclosed, this method is to be raw material with trivalent iron salt iron nitrate, phosphoric acid, lithium acetate, obtains spherical LiFePO 4 by sol-gel method.The iron lithium phosphate median size that this method is prepared is 5-8um, and tap density can reach 1.8-2.0g/cm
3, first discharge specific capacity can reach 140-160mAh/g under the room temperature.
Summary of the invention
Purpose of the present invention is exactly in order to overcome and to avoid the shortcoming and defect of prior art and the preparation method that a kind of technology is simple, with low cost, microwave sintering legal system that be suitable for producing is equipped with high-performance iron phosphate lithium is provided, and the present invention adopts following technical measures to realize its purpose.
Be the 0.2-2 mol with concentration of iron earlier, phosphorus concentration is a phosphorus: iron=(1.1-2,0): 1 (mol ratio), complexing agent concentration is a complexing agent: iron=(0.01-0,3): the ferrous sulfate of 1 (mol ratio), phosphorus source, complexing agent mixed aqueous solution and concentration are the ammonia soln reaction synthesizing spherical ferrous ammonium phosphate presoma of 2-10 mol, dry back of washing and Quilonum Retard add proper amount of carbon source with 1: 1 uniform mixing of mol ratio; Dry back with 10-40MPa pressure compressing tablet, is imbedded then to fill with and is used for absorbing microwave and produces in the crucible of carbon of protective atmosphere on tabletting machine; Crucible is put into microwave oven to be heated 1-20 minute under the 100W-800W microwave power; The heating relief crucible that finishes naturally cools to room temperature and obtains spherical LiFePO 4.The gained LiFePO 4 powder is a spheroidal particle, tap density height, good conductivity, specific storage height.
Described phosphorus source is one or more in phosphoric acid, primary ammonium phosphate and the Secondary ammonium phosphate.
Described complexing agent is one or more in citric acid and the tartrate.
In the process of described synthesizing spherical ferrous ammonium phosphate presoma, the temperature of controlling reactor internal reaction liquid is 45-90 ℃, and the pH value of controlling reactor internal reaction liquid is 5.0-8.0.
Described carbon source is one or more in carbon black, acetylene black, sucrose, starch, the gac.
The described carbon that is used for absorbing microwave and produces protective atmosphere is one or more in graphite, the activated carbon.
The concentration of described ammonia soln is the 2-10 mol.
At synthesizing spherical ferrous ammonium phosphate (NH
4FePO
4H
2O) in the process of presoma, the temperature of controlling reactor internal reaction liquid is 45-90 ℃.120 milliliters in constant ferrous sulfate, phosphorus source, complexing agent mixed aqueous solution/time flow, regulate the flow of ammonia soln simultaneously, make the pH value of reactor internal reaction liquid be 5.0-8.0.
The total concn of iron and manganese is the 0.2-2 mol in described ferrous sulfate, manganous sulfate, phosphorus source, the complexing agent mixed aqueous solution, wherein 0＜(manganese/(iron+manganese)≤40% (molar percentage).
Phosphorus source in described ferrous sulfate, manganous sulfate, phosphorus source, the complexing agent mixed aqueous solution is one or more in phosphoric acid, primary ammonium phosphate and the Secondary ammonium phosphate, and the concentration of phosphorus is phosphorus in the aqueous solution: (iron+manganese)=(1.1-2): 1 (mol ratio).
The concentration of described ammonia soln is the 2-10 mol.
The invention has the beneficial effects as follows that it is 7-12um that this preparation method prepares median size, tap density can reach 2.0-2.2g/cm3, and first discharge specific capacity can reach the high-bulk-density of 145-160mAh/g, the lithium ion battery anode material spherical LiFePO 4 of high-volume and capacity ratio under the room temperature.Compare with the trivalent iron salt route; the present invention utilizes divalent iron salt to be raw material; raw material sources are more extensive; be easy to improve material lithium ion specific conductivity and actual capacity by mixing manganese; need not a large amount of carbon source reduction ferric ions during thermal treatment; protective atmosphere is required to reduce, have certain advantage, very with practical value.
Embodiment
The specific implementation method of preparation high-density spherical ferric lithium phosphate (LiFePO4) comprises following each step successively:
1. prepare ferrous sulfate, phosphorus source, complexing agent mixed aqueous solution, wherein the concentration of iron is the 0.2-2 mol, and the concentration of phosphorus is phosphorus: iron two (1.1-2): 1 (mol ratio), complexing agent concentration are complexing agent: iron=(0.01-0.3): 1 (mol ratio).
2. compound concentration is the ammonia soln of 2-10 mol.
3. with above-mentioned ferrous sulfate, phosphorus source, complexing agent mixed aqueous solution, ammonia soln is input to respectively in the reactor of band stirring continuously with pump, and the temperature of controlling reactor internal reaction liquid is 45-90 ℃.The flow that constant ferrous sulfate, phosphorus source, complexing agent mixed aqueous solution are 120 milliliters/hour is regulated the flow of ammonia soln simultaneously, makes the pH value of reactor internal reaction liquid be 5.0-8.0.Mixture nature overflow in the reactor is discharged.
4. step (3) gained material is changed over to and carry out solid-liquid separation in the solid-liquid separator, with the solid product of deionized water washing solid-liquid separation gained, until the SO that can not detect with BaCl2 in the washing water
4 2-Till.Product after the washing in 80-100 ℃ of dry 2-4 hour, gets spherical ferrous ammonium phosphate in moisture eliminator.
5. by Li: Fe: P=1: 1: 1 mol ratio takes by weighing spherical ferrous ammonium phosphate and Quilonum Retard and adds water and mix, and adds the conduction carbon source, and decomposing afterwards, the residual carbon quality is 1～20wt% of iron lithium phosphate.The heating evaporating water.
On tabletting machine with 10-40Mpa pressure compressing tablet.The every tablet quality of material is between the 1-10 gram.
7. step 6 products therefrom is imbedded to fill with and be used for absorbing in the crucible of microwave and the carbon that produces protective atmosphere material: carbon=(0.1-1): 1 (mass ratio).
8. crucible is put into microwave oven heats 1-60 minute with 100-800W.Heat the relief crucible that finishes and naturally cool to room temperature.Obtain spherical LiFePO 4
In above-mentioned preparation method's step (1), described phosphorus source is one or more in phosphoric acid, primary ammonium phosphate, the Secondary ammonium phosphate.
In above-mentioned preparation method's step (1), described complexing agent is one or more in citric acid, the tartrate.
Introduce embodiments of the invention below:
Embodiment 1
Preparation ferrous sulfate, phosphoric acid, citric acid mixed aqueous solution, wherein ferrous sulfate concentration is that 1.5 mol, phosphoric acid concentration are that 2,25 mol, citric acid concentration are 0.15 mol.Compound concentration is the ammonia soln of 10 mol.Respectively ferrous sulfate, phosphoric acid, citric acid mixed aqueous solution and ammonia soln are input to volume pump in the reactor of 3 liter capacities that filled with deionized water in advance and react, the flow of control ferrous sulfate, phosphoric acid, citric acid mixed aqueous solution be 120 milliliters/time, regulate the flow of ammonia soln, the pH value of controlling reactor internal reaction liquid is 5.0 ± 0.1.Temperature is 80-C in the controlling reactor.Mixture nature overflow in the reactor enters in the receiving tank.After the continuously feeding 30 hours, stop charging, the material in the reactor is discharged, carry out solid-liquid separation with whizzer.With the solid product of 60 ℃ deionized waters washing solid-liquid separation gained, until using BaCl: can not detect SO+ ' in the washing water-till.With the product after the washing in loft drier in 80 ℃ dry 3 hours down, obtain spherical ferrous ammonium phosphate.Take by weighing 18.5 the gram Quilonum Retards (": CO.) and measure 18.5 milliliters of deionized waters, place the ball mill ball milling to stop after 3 hours.Take by weighing the above-mentioned ferrous ammonium phosphate that makes of 93.5 grams, place the Quilonum Retard slurry behind the ball milling, slowly stirred 10 minutes, obtain mixed slurry.Mixed slurry is put into alumina crucible, speed by 200 ℃/hour in tube furnace is warming up to 800 ℃, constant temperature 16 hours, stop heating, in stove, naturally cool to room temperature, continue in the tube furnace to feed nitrogen in this process, gas flow is 1 liter/minute, obtains the spherical LiFePO 4 product.Recording this product median size is 8-10um, and tap density is 2.05g/cm '.With the lithium sheet is negative pole, and recording this iron lithium phosphate first discharge specific capacity at room temperature is 150mAh/go
Embodiment 2
Preparation ferrous sulfate, primary ammonium phosphate, tartrate mixed aqueous solution, wherein ferrous sulfate concentration is that 0.5 mol, biphosphate ammonium concentration are that 0.6 mol, tartaric acid concentration are 0.1 mol.Compound concentration is the ammonia soln of 2 mol.Respectively ferrous sulfate, phosphoric acid, tartrate mixed aqueous solution and ammonia soln are input to volume pump in the reactor of 3 liter capacities that filled with deionized water in advance and react, the flow of control ferrous sulfate, phosphoric acid, tartrate mixed aqueous solution be 120 milliliters/time, regulate the flow of ammonia soln, the pH value of controlling reactor internal reaction liquid is 6.5 ± 0.1.Temperature is 70 ℃ in the controlling reactor.Mixture nature overflow in the reactor enters in the receiving tank.After the continuously feeding 30 hours, stop charging, the material in the reactor is discharged, carry out solid-liquid separation with whizzer.With the solid product of 60 ℃ deionized water washing solid-liquid separation gained, until using BaCl: can not detect till the SO42-in the washing water.With the product after the washing in loft drier in 80 ℃ dry 3 hours down, obtain spherical ferrous ammonium phosphate.(Li, CO: the people is also measured 18.5 milliliters of deionized waters, places the ball mill ball milling to stop after 3 hours to take by weighing 18.5 gram Quilonum Retards.Take by weighing the above-mentioned ferrous ammonium phosphate that makes of 93.5 grams, place the Quilonum Retard slurry behind the ball milling, slowly stirred 10 minutes, obtain mixed slurry.Mixed slurry is put into alumina crucible, in tube furnace by 200 ℃/time speed be warming up to 800 ℃, constant temperature 16 hours, stop heating, in stove, naturally cool to room temperature, in this process, continue to feed nitrogen in the tube furnace, gas flow is 1 liter/minute, obtains the spherical LiFePO 4 product.Recording this product median size is 7-9 ware m, and tap density is 2.01g/em3.With the lithium sheet is negative pole, and recording this iron lithium phosphate first discharge specific capacity at room temperature is 150mAh/g.
Embodiment 3
Replace the phosphoric acid of 2.25 mol with the Secondary ammonium phosphate of 2,25 mol, prepare spherical LiFePO 4 by embodiment 1 identical condition.Recording this product median size is 8-10L1m, and tap density is 2,05g/cm '.With the lithium sheet is negative pole, and recording this iron lithium phosphate first discharge specific capacity at room temperature is 150mAh/S.
Embodiment, 4
Preparation ferrous sulfate, manganous sulfate, phosphoric acid, citric acid mixed aqueous solution, wherein ferrous sulfate concentration is that 1.2 mol, manganous sulfate concentration are that 0.3 mol, phosphoric acid concentration are that 2.25 mol, citric acid concentration are 0.15 mol.Compound concentration is the ammonia soln of 8 mol.Respectively ferrous sulfate, manganous sulfate, phosphoric acid, citric acid mixed aqueous solution and ammonia soln are input to volume pump in the reactor of 3 liter capacities that filled with deionized water in advance and react, the flow of control ferrous sulfate, manganous sulfate, phosphoric acid, citric acid mixed aqueous solution be 120 milliliters of rivers, the time, regulate the flow of ammonia soln, the pH value of controlling reactor internal reaction liquid is 7,0 ± 0.1.Temperature is 80 ℃ in the controlling reactor.Mixture nature overflow in the reactor enters in the receiving tank.After the continuously feeding 30 hours, stop charging, the material in the reactor is discharged, carry out solid-liquid separation with whizzer.With the solid product of 60 ℃ deionized water washing solid-liquid separation gained, until using BaCl: can not detect till the SOft in the washing water.With the product after the washing in loft drier in 80 ℃ dry 3 hours down, obtain spherical manganous phosphate ferrous ammonium (NH4Fe ()..Mno.。PO4●H:O)。Take by weighing 18.5 gram Quilonum Retards (Li2CO3) and measure 18.5 milliliters of deionized waters, place the ball mill ball milling to stop after 3 hours.Take by weighing the above-mentioned manganous phosphate ferrous ammonium that makes of 93.5 grams, place the Quilonum Retard slurry behind the ball milling, slowly stirred 10 minutes, obtain mixed slurry.
Mixed slurry is put into alumina crucible, speed by 200 ℃/hour in tube furnace is warming up to 800 ℃, constant temperature 16 hours, stop heating, in stove, naturally cool to room temperature, continue in the tube furnace to feed nitrogen in this process, gas flow is 1 liter/minute, obtains spherical iron manganese phosphate for lithium (LiFeo..Mno.:PO4) product.Recording this product median size is 8-101jm, and tap density is 2.08g/cm3.With the lithium sheet is negative pole, and recording this iron manganese phosphate for lithium first discharge specific capacity at room temperature is 155mAh/g.
Embodiment 5
Preparation ferrous sulfate, manganous sulfate, phosphoric acid, citric acid mixed aqueous solution, wherein ferrous sulfate concentration is that 0.9 mol, manganous sulfate concentration are that 0.6 mol, phosphoric acid concentration are that 2.25 mol, citric acid concentration are 0,15 mol.Compound concentration is the ammonia soln of 6 mol.Respectively ferrous sulfate, manganous sulfate, phosphoric acid, citric acid mixed aqueous solution and ammonia soln are input to volume pump in the reactor of 3 liter capacities that filled with deionized water in advance and react, the flow of control ferrous sulfate, manganous sulfate, phosphoric acid, citric acid mixed aqueous solution is 120 milliliters/hour, regulate the flow of ammonia soln, the pH value of controlling reactor internal reaction liquid is 8.0 ± 0.1.Temperature is 80 ℃ in the controlling reactor.Mixture nature overflow in the reactor enters in the receiving tank.After the continuously feeding 30 hours, stop charging, the material in the reactor is discharged, carry out solid-liquid separation with whizzer.With the solid product of 60 ℃ deionized water washing solid-liquid separation gained, until using BaCl: can not detect the SO4 in the washing water
2-Till.With the product after the washing in loft drier in 80 ℃ dry 3 hours down, obtain spherical manganous phosphate ferrous ammonium (NH4Fe ()..Mno.+PO4.H
2O)。Take by weighing 18.5 gram Quilonum Retards (" ￡ 0:1) and measure 18.5 milliliters of deionized waters, place the ball mill ball milling to stop after 3 hours.Take by weighing the above-mentioned manganous phosphate ferrous ammonium that makes of 93.5 grams, place the Quilonum Retard slurry behind the ball milling, slowly stirred 10 minutes, obtain mixed slurry.Mixed slurry is put into alumina crucible, speed by 200 ℃/hour in tube furnace is warming up to 800 ℃, constant temperature 16 hours, stop heating, in stove, naturally cool to room temperature, continue in the tube furnace to feed nitrogen in this process, gas flow is 1 liter/minute, obtains spherical iron manganese phosphate for lithium (" Feo..Mno.4PO4) product.Recording this product median size is 8-10um, and tap density is 2.10g/cm3.With the lithium sheet is negative pole, and recording this iron manganese phosphate for lithium first discharge specific capacity at room temperature is 160mAh/g.
Embodiment 6
Thermal treatment temp is 900 ℃, constant temperature 48 hours, and other condition obtains spherical iron manganese phosphate for lithium ((one) Fec) friend n with embodiment 5.., PO) product.Recording this product median size is 7-9vm, and tap density is 2.20g/cm '.With the lithium sheet is negative pole, and recording this iron manganese phosphate for lithium first discharge specific capacity at room temperature is 147Mh/go.
Claims (6)
1. microwave sintering method for preparing high-performance iron phosphate lithium, it is characterized in that being the 0.2-2 mol with concentration of iron earlier, phosphorus concentration is a phosphorus: iron=(1.1-2,0): 1 (mol ratio), complexing agent concentration is a complexing agent: iron=(0.01-0,3): the ferrous sulfate of 1 (mol ratio), phosphorus source, complexing agent mixed aqueous solution and concentration are the ammonia soln reaction synthesizing spherical ferrous ammonium phosphate presoma of 2-10 mol, dry back of washing and Quilonum Retard add proper amount of carbon source with 1: 1 uniform mixing of mol ratio; Dry back with 10-40MPa pressure compressing tablet, is imbedded then to fill with and is used for absorbing microwave and produces in the crucible of carbon of protective atmosphere on tabletting machine; Crucible is put into microwave oven to be heated 1-20 minute under the 100W-800W microwave power; The heating relief crucible that finishes naturally cools to room temperature and obtains spherical LiFePO 4.
2. a kind of microwave sintering method for preparing high-performance iron phosphate lithium according to claim 1 is characterized in that described phosphorus source is one or more in phosphoric acid, primary ammonium phosphate and the Secondary ammonium phosphate.
3. a kind of microwave sintering method for preparing high-performance iron phosphate lithium according to claim 2 is characterized in that described complexing agent is one or more in citric acid and the tartrate.
4. according to the described a kind of microwave sintering method for preparing high-performance iron phosphate lithium of claim 3, it is characterized in that in the process of described synthesizing spherical ferrous ammonium phosphate presoma, the temperature of controlling reactor internal reaction liquid is 45-90 ℃, and the pH value of controlling reactor internal reaction liquid is 5.0-8.0.
5. a kind of microwave sintering method for preparing high-performance iron phosphate lithium according to claim 4 is characterized in that described carbon source is one or more in carbon black, acetylene black, sucrose, starch, the gac.
6. a kind of microwave sintering method for preparing high-performance iron phosphate lithium according to claim 5 is characterized in that the described carbon that is used for absorbing microwave and produces protective atmosphere is one or more in graphite, the activated carbon.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102214820A (en) * | 2011-01-14 | 2011-10-12 | 王世宏 | Industrial preparation method for multielement-coated lithium manganese oxide material |
| CN104409734A (en) * | 2014-12-26 | 2015-03-11 | 北京化工大学 | Lithium iron phosphate battery positive material prepared by using microwave-assisted sol-gel method |
| CN106099103A (en) * | 2016-08-24 | 2016-11-09 | 合肥国轩电池材料有限公司 | A kind of preparation method of low-cost and high-performance LiFePO 4 material |
| CN111348638A (en) * | 2020-05-11 | 2020-06-30 | 蒋达金 | Preparation method of basic ammonium ferric phosphate |
| CN113044822A (en) * | 2021-02-07 | 2021-06-29 | 桂林理工大学 | Method for preparing high-conductivity iron phosphate in situ by utilizing space limited domain of waste sponge |
-
2009
- 2009-10-14 CN CN200910019319A patent/CN101759172A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102214820A (en) * | 2011-01-14 | 2011-10-12 | 王世宏 | Industrial preparation method for multielement-coated lithium manganese oxide material |
| CN104409734A (en) * | 2014-12-26 | 2015-03-11 | 北京化工大学 | Lithium iron phosphate battery positive material prepared by using microwave-assisted sol-gel method |
| CN106099103A (en) * | 2016-08-24 | 2016-11-09 | 合肥国轩电池材料有限公司 | A kind of preparation method of low-cost and high-performance LiFePO 4 material |
| CN111348638A (en) * | 2020-05-11 | 2020-06-30 | 蒋达金 | Preparation method of basic ammonium ferric phosphate |
| CN111348638B (en) * | 2020-05-11 | 2021-07-06 | 蒋达金 | Preparation method of basic ammonium ferric phosphate |
| CN113044822A (en) * | 2021-02-07 | 2021-06-29 | 桂林理工大学 | Method for preparing high-conductivity iron phosphate in situ by utilizing space limited domain of waste sponge |
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Application publication date: 20100630 |