CN102838102A - Preparation method of lithium iron phosphate monocrystalline nanorods - Google Patents
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Abstract
The invention relates to a preparation method of lithium iron phosphate monocrystalline nanorods. The method is characterized in that: mixed solvent required by solvothermal reaction is constituted by ethylene glycol and water at volume ratio of 3:1-1:3; and polyethylene glycol is introduced to influence crystal nucleus formation and crystal growth, and realize solvothermal synthesis of lithium iron phosphate monocrystalline nanorods. The preparation method includes dissolving antioxidant ascorbic acid in the mixed solvent of ethylene glycol and water; sequentially dissolving phosphoric acid and ferrous sulfate hexahydrate in the mixed solvent; dropwise adding lithium hydroxide dissolved in ethylene glycol and water into the above solution containing phosphoric acid, ferrous sulfate and ascorbic acid; mixing with appropriate amount of polyethylene glycol; sealing in a reaction kettle system; and performing solvothermal reaction under high temperature 160-240 DEG C and high pressure, to obtain lithium iron phosphate monocrystalline nanorods. The product has stable quality, high purity and good particle dispersivity, which facilitates lithium ion diffusion and improves electrochemical performance of lithium ion battery. The preparation method has the advantages of simple preparation process, easy control, no pollution, low cost, and easy mass production.
Description
Technical field
The present invention relates to a kind of preparation method of iron lithium phosphate monocrystal nano rod, belong to ceramic, energy-storage battery field of materials.
Background technology
Lithium ion battery is as a kind of high performance green power supply of filling; In various portable type electronic products and communication tool, be used widely in recent years; And progressively be developed as the electrical source of power of electromobile, develop thereby promote its direction to safety, environmental protection, low cost and high-energy-density.Wherein, particularly the development of positive electrode material is very crucial for the novel electrode material.The anode material for lithium-ion batteries of broad research concentrates on the transition metal oxide of lithium such as the LiMO of laminate structure at present
2(M=Co, Ni is Mn) with the LiMn of spinel structure
2O
4But they respectively have shortcoming, LICoO as positive electrode material
2Cost is high, natural resources shortage, and toxicity is big; Lithium nickelate (LiNiO
2) the preparation difficulty, poor heat stability; LIMn
2O
4Capacity is lower, and cyclical stability especially high-temperature behavior is relatively poor.In order to solve the defective of above material, battery circle has been done big quantity research, above positive electrode material is being carried out various modifications with when improving its performance, and the exploitation of novel anode material also is the emphasis of paying close attention to always.Discover; LiFePO 4 material WV moderate (3.4V), platform are good, the high 170mAh/g of theoretical capacity, and cycle performance is superior; Cost is very low; Its high-energy-density and high safety performance make it in power lithium-ion battery, have outstanding application prospect, and weak point is that its poorly conductive and lithium ion velocity of diffusion is slow, and the microscopic appearance of this and lithium iron phosphate positive material has great related.At present, academia still is in the stage that proposes hypothesis to the concrete mechanism and the process of iron lithium phosphate removal lithium embedded, is difficult to through experimental verification.The lithium iron phosphate positive material of industrialization at present basically all is that high temperature solid-state method is synthetic, and microscopic appearance is spherical, inquires about through document; The iron lithium phosphate microscopic appearance of preparation still is difficult to regulation and control in the laboratory; Concentrate on the block and spherical of diamond pattern, for example (nature. 2009,458 for the positive electrode material of people's high temperature solid-state method preparation such as Kang Byoungwoo; 190.); Or people such as Yang SF are spherical through the iron lithium phosphate (ELECTROCHEMISTRY COMMUNICATIONS. 2001,3,505.) of Hydrothermal Preparation; More than the neither energy density that promotes lithium ion battery that is beneficial to, and make and be difficult to realize through the dynamic change of observation procedures such as original position TEM research positive electrode material crystalline structure.
Summary of the invention
Deficiency to prior art exists the object of the present invention is to provide a kind of technology simple, the preparation method of the iron lithium phosphate monocrystal nano rod that is easy to control.
The preparation method of iron lithium phosphate monocrystal nano rod of the present invention, employing be the solvent thermal synthesis method, may further comprise the steps:
1), obtains the mixed solvent of terepthaloyl moietie and water with terepthaloyl moietie and deionized water 3:1 ~ 1:3 mixing by volume;
2) xitix is dissolved in the mixed solvent of terepthaloyl moietie and water of step 1), is stirred to abundant dissolving, obtain ascorbic acid solution;
3) mol ratio by P and Fe is 1:1; Metering takes by weighing phosphoric acid and six directions aqueous ferrous sulfate; And phosphoric acid and six directions aqueous ferrous sulfate being dissolved in step 2) in the prepared ascorbic acid solution, xitix quality and prepared target iron lithium phosphate mass percent are 10 ~ 30%, the concentration of phosphoric acid and six directions aqueous ferrous sulfate is 0.05 ~ 0.5mol/L; Fully stir, obtain containing the solution of phosphoric acid, ferrous sulfate and xitix;
The amount of the phosphoric acid that 4) takes by weighing according to step 3) is 3:1 by the mol ratio of Li and P, and metering takes by weighing Lithium Hydroxide MonoHydrate; And Lithium Hydroxide MonoHydrate is dissolved in the mixed solvent of terepthaloyl moietie and water of step 1); The concentration that makes Lithium Hydroxide MonoHydrate is 0.15 ~ 1.5mol/L, fully stirs, and obtains lithium hydroxide solution;
5) under the state that stirs, the lithium hydroxide solution of step 4) is added drop-wise in the prepared solution that contains phosphoric acid, ferrous sulfate and xitix of step 3), forms and contain sedimentary suspension-s;
6) stir down, polyoxyethylene glycol is added in the suspension-s of step 5), polyoxyethylene glycol quality and prepared target iron lithium phosphate mass percent are 10 ~ 100%; Transfer to then in the autoclave, regulate, make its volume account for reaction kettle inner bag volumetrical 2/3 ~ 4/5 with the mixed solvent that step 1) is prepared; Continue to stir at least 5 minutes, airtight, after being incubated 4 ~ 36 hours under 160 ~ 240 ℃; Reduce to room temperature, take out reaction product, filter; Use deionized water, absolute ethyl alcohol or acetone successively, dry under 40 ℃ ~ 100 ℃ temperature, obtain the iron lithium phosphate monocrystal nano rod.
Among the present invention, the purity of said phosphoric acid, six directions ferrous sulfate, Lithium Hydroxide MonoHydrate, xitix, polyoxyethylene glycol, terepthaloyl moietie, absolute ethyl alcohol and acetone all is not less than CP.
The radial dimension of the iron lithium phosphate monocrystal nano rod that the inventive method is prepared is the 50-200 nanometer, and length is the 0.5-10 micron.
The present invention is a reaction solvent with the mixed solvent of terepthaloyl moietie and water; Volume ratio through terepthaloyl moietie and water in the design mixed solvent; In conjunction with the finishing effect of polyoxyethylene glycol, coring and process of growth in the regulation and control heat treatment process realize that the solvent thermal of iron lithium phosphate monocrystal nano rod is synthetic.Adopt the dehydration of absolute ethyl alcohol and acetone, and be not higher than 100
oThe oven dry of C is in order to obtain the iron lithium phosphate monocrystal nano rod of good dispersibility.
The constant product quality that the inventive method makes, purity is high, and particles dispersed property is good, helps the lithium ion diffusion, improves the large current density performance of lithium ion battery.Preparation process of the present invention is simple, is easy to control, and pollution-free, cost is low, is easy to large-scale production.
Description of drawings
X-ray diffraction (XRD) collection of illustrative plates of Fig. 1 synthetic iron lithium phosphate of the present invention monocrystal nano rod;
Sem (SEM) photo of Fig. 2 synthetic iron lithium phosphate of the present invention monocrystal nano rod;
High resolution transmission electron microscopy (HRTEM) photo of Fig. 3 iron lithium phosphate monocrystal nano rod of the present invention;
The charging and discharging curve of the lithium ion battery that Fig. 4 synthetic iron lithium phosphate of the present invention monocrystal nano rod is assembled as positive electrode material after covering carbon thermal treatment.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Instance 1
The preparation method may further comprise the steps:
1) measures terepthaloyl moietie 20ml and deionized water 20ml, with the mixed solvent of the two mixed preparing terepthaloyl moietie and water.
2) metering takes by weighing xitix 0.1g and is dissolved in the mixed solvent of prepared terepthaloyl moietie of step 1) and water, stirs it fully to be dissolved in 30 minutes.
3) mol ratio by P and Fe is 1:1; Metering takes by weighing phosphoric acid 0.4612g, six directions aqueous ferrous sulfate 1.1121g is dissolved in step 2) in the prepared ascorbic acid solution; Stirred 10 minutes, and obtained containing the solution of phosphoric acid, ferrous sulfate and xitix, xitix accounts for 15.8% of target iron lithium phosphate quality; Phosphoric acid concentration is 0.1mol/L, and six directions aqueous ferrous sulfate concentration is 0.1mol/L.
The amount of the phosphoric acid that 4) takes by weighing according to step 3) is 3:1 by the mol ratio of Li and P, and metering takes by weighing Lithium Hydroxide MonoHydrate 0.5035g; Be dissolved in the mixed solvent of prepared terepthaloyl moietie of step 1) and water; Stirred 30 minutes, and joined to such an extent that clarify lithium hydroxide solution, the concentration of Lithium Hydroxide MonoHydrate is 0.3mol/L.
5) under the state that stirs, the lithium hydroxide solution that step 4) is prepared is added drop-wise in the prepared solution that contains phosphoric acid, ferrous sulfate and xitix of step 3), forms to contain sedimentary suspension-s.After mixing completion, stirred 30 minutes.
6) stir down, the 0.0631g polyoxyethylene glycol is added in the prepared suspension-s of step 5), transfer to again in the autoclave, regulate, make its volume account for reaction kettle inner bag volumetrical 4/5, continue to stir 10 minutes with the mixed solvent that step 1) is prepared.Airtight, be incubated 6 hours down at 200 ℃ and heat-treat.Then, reduce to room temperature, take out reaction product, filter, use deionized water, acetone successively, dry under 80 ℃ of temperature, obtain the iron lithium phosphate monocrystal nano rod.
Its X-ray diffraction (XRD) collection of illustrative plates is seen Fig. 1, and visible by figure, crystalline phase is shown as pure phase, inclusion-free, and crystalline structure is complete.
Microscopic appearance is single, and scantlings of the structure is comparatively concentrated, is monocrystal nano rod, and radial dimension is the 50-100 nanometer, and length is 0.5-5 micron (seeing Fig. 2, Fig. 3).
The iron lithium phosphate monocrystal nano rod is made the chemical property of lithium ion battery:
The iron lithium phosphate monocrystal nano rod that this example is made is poured into to mix in the 20ml deionized water of the xitix that is dissolved with 0.15g and was stirred 30 minutes; 80 ℃ of dryings are taken out after 12 hours and are carried out anneal in the baking oven; 600 ℃ of following nitrogen protective sintering 6 hours obtain the lithium iron phosphate positive material powder after the grinding.This lithium iron phosphate positive material powder, acetylene black and pvdf prepared by mass ratio (75:15:10) and fully stir it is uniformly dispersed; With the N-Methyl pyrrolidone is to be applied on the aluminium foil behind the solvent furnishing pulpous state, in vacuum drying oven 100 ℃ down behind the dry 12h cut-parts become positive plate.As negative pole, cel-gard 2000 microporous membranes are as diaphragm with metal lithium sheet, and the LiPF of 1 mol/L (99.9%, solvent is ethylene carbonate and the dimethyl carbonate mixed solution of volume ratio 1:1) is an electrolytic solution, at water-content less than 0.1 * 10
-6Glove box in successively positive plate, barrier film, negative plate, nickel foam and negative cover are put into anode cover from bottom to top and compress and be made into button cell, and it is carried out charge-discharge test.Cover after the carbon thermal treatment lithium ion battery with synthetic iron lithium phosphate monocrystal nano rod as the positive electrode material assembling; Good cycling stability; Life-span is long; High rate performance is very excellent, carries out charge-discharge test with the electric current of 170mA/g (current density=1C), obtains the excellent capacity of 141 mAh/g.Fig. 4 synthetic iron lithium phosphate of the present invention monocrystal nano rod covers after the carbon thermal treatment charging and discharging curve as the lithium ion battery of positive electrode material assembling.
1) measures terepthaloyl moietie 40ml and deionized water 40ml, with the mixed solvent of the two mixed preparing terepthaloyl moietie and water.
2) metering takes by weighing xitix 0.063g and is dissolved in the mixed solvent of prepared terepthaloyl moietie of step 1) and water, stirs it fully to be dissolved in 30 minutes.
3) mol ratio by P and Fe is 1:1; Metering takes by weighing phosphoric acid 0.4612g, six directions aqueous ferrous sulfate 1.1121g is dissolved in step 2) in the prepared ascorbic acid solution; Stirred 10 minutes, and obtained containing the solution of phosphoric acid, ferrous sulfate and xitix, xitix accounts for 10% of target iron lithium phosphate quality; Phosphoric acid concentration is 0.05mol/L, and six directions aqueous ferrous sulfate concentration is 0.05mol/L.
The amount of the phosphoric acid that 4) takes by weighing according to step 3) is 3:1 by the mol ratio of Li and P, and metering takes by weighing Lithium Hydroxide MonoHydrate 0.5035g; Be dissolved in the mixed solvent of prepared terepthaloyl moietie of step 1) and water; Stirred 30 minutes, and joined to such an extent that clarify lithium hydroxide solution, the concentration of Lithium Hydroxide MonoHydrate is 0.15mol/L.
5) under the state that stirs, the lithium hydroxide solution that step 4) is prepared is added drop-wise in the prepared solution that contains phosphoric acid, ferrous sulfate and xitix of step 3), forms to contain sedimentary suspension-s.After mixing completion, stirred 30 minutes.
6) stir down, the 0.316g polyoxyethylene glycol is added in the prepared suspension-s of step 5), transfer to again in the autoclave, regulate, make its volume account for reaction kettle inner bag volumetrical 4/5, continue to stir 10 minutes with the mixed solvent that step 1) is prepared.Airtight, be incubated 6 hours down at 240 ℃ and heat-treat.Then, reduce to room temperature, take out reaction product, filter, use deionized water, acetone successively, dry under 80 ℃ of temperature, obtain the iron lithium phosphate monocrystal nano rod.Radial dimension is the 100-200 nanometer, and length is the 1-5 micron
Instance 3
1) measures terepthaloyl moietie 20ml and deionized water 20ml, with the mixed solvent of the two mixed preparing terepthaloyl moietie and water.
2) metering takes by weighing xitix 0.189g and is dissolved in the mixed solvent of prepared terepthaloyl moietie of step 1) and water, stirs it fully to be dissolved in 30 minutes.
3) mol ratio by P and Fe is 1:1; Metering takes by weighing phosphoric acid 0.4612g, six directions aqueous ferrous sulfate 1.1121g is dissolved in step 2) in the prepared ascorbic acid solution; Stirred 10 minutes, and obtained containing the solution of phosphoric acid, ferrous sulfate and xitix, xitix accounts for 30% of target iron lithium phosphate quality; Phosphoric acid concentration is 0.1mol/L, and six directions aqueous ferrous sulfate concentration is 0.1mol/L.
The amount of the phosphoric acid that 4) takes by weighing according to step 3) is 3:1 by the mol ratio of Li and P, and metering takes by weighing Lithium Hydroxide MonoHydrate 0.5035g; Be dissolved in the mixed solvent of prepared terepthaloyl moietie of step 1) and water; Stirred 30 minutes, and joined to such an extent that clarify lithium hydroxide solution, the concentration of Lithium Hydroxide MonoHydrate is 0.3mol/L.
5) under the state that stirs, the lithium hydroxide solution that step 4) is prepared is added drop-wise in the prepared solution that contains phosphoric acid, ferrous sulfate and xitix of step 3), forms to contain sedimentary suspension-s.After mixing completion, stirred 30 minutes.
6) stir down, the 0.631g polyoxyethylene glycol is added in the prepared suspension-s of step 5), transfer to again in the autoclave, regulate, make its volume account for reaction kettle inner bag volumetrical 4/5, continue to stir 10 minutes with the mixed solvent that step 1) is prepared.Airtight, be incubated 36 hours down at 160 ℃ and heat-treat.Then, reduce to room temperature, take out reaction product, filter, use deionized water, acetone successively, dry under 80 ℃ of temperature, obtain the iron lithium phosphate monocrystal nano rod, radial dimension is the 100-200 nanometer, and length is the 5-10 micron.
Instance 4
1) measures terepthaloyl moietie 20ml and deionized water 20ml, with the mixed solvent of the two mixed preparing terepthaloyl moietie and water.
2) metering takes by weighing xitix 0.5g and is dissolved in the mixed solvent of prepared terepthaloyl moietie of step 1) and water, stirs it fully to be dissolved in 30 minutes.
3) mol ratio by P and Fe is 1:1; Metering takes by weighing phosphoric acid 2.306g, six directions aqueous ferrous sulfate 5.5605g is dissolved in step 2) in the prepared ascorbic acid solution; Stirred 10 minutes, and obtained containing the solution of phosphoric acid, ferrous sulfate and xitix, xitix accounts for 15.8% of target iron lithium phosphate quality; Phosphoric acid concentration is 0.5mol/L, and six directions aqueous ferrous sulfate concentration is 0.5mol/L.
The amount of the phosphoric acid that 4) takes by weighing according to step 3) is 3:1 by the mol ratio of Li and P, and metering takes by weighing Lithium Hydroxide MonoHydrate 2.5175g; Be dissolved in the mixed solvent of prepared terepthaloyl moietie of step 1) and water; Stirred 30 minutes, and joined to such an extent that clarify lithium hydroxide solution, the concentration of Lithium Hydroxide MonoHydrate is 1.5mol/L.
5) under the state that stirs, the lithium hydroxide solution that step 4) is prepared is added drop-wise in the prepared solution that contains phosphoric acid, ferrous sulfate and xitix of step 3), forms to contain sedimentary suspension-s.After mixing completion, stirred 30 minutes.
6) stir down, the 0.0631g polyoxyethylene glycol is added in the prepared suspension-s of step 5), transfer to again in the autoclave, regulate, make its volume account for reaction kettle inner bag volumetrical 2/3, continue to stir 10 minutes with the mixed solvent that step 1) is prepared.Airtight, be incubated 24 hours down at 200 ℃ and heat-treat.Then, reduce to room temperature, take out reaction product, filter, use deionized water, acetone successively, dry under 80 ℃ of temperature, obtain the iron lithium phosphate monocrystal nano rod, radial dimension is the 50-100 nanometer, and length is the 2-8 micron.
Claims (3)
1. the preparation method of an iron lithium phosphate monocrystal nano rod is characterized in that may further comprise the steps:
1), obtains the mixed solvent of terepthaloyl moietie and water with terepthaloyl moietie and deionized water 3:1 ~ 1:3 mixing by volume;
2) xitix is dissolved in the mixed solvent of terepthaloyl moietie and water of step 1), is stirred to abundant dissolving, obtain ascorbic acid solution;
3) mol ratio by P and Fe is 1:1; Metering takes by weighing phosphoric acid and six directions aqueous ferrous sulfate; And phosphoric acid and six directions aqueous ferrous sulfate being dissolved in step 2) in the prepared ascorbic acid solution, xitix quality and prepared target iron lithium phosphate mass percent are 10 ~ 30%, the concentration of phosphoric acid and six directions aqueous ferrous sulfate is 0.05 ~ 0.5mol/L; Fully stir, obtain containing the solution of phosphoric acid, ferrous sulfate and xitix;
The amount of the phosphoric acid that 4) takes by weighing according to step 3) is 3:1 by the mol ratio of Li and P, and metering takes by weighing Lithium Hydroxide MonoHydrate; And Lithium Hydroxide MonoHydrate is dissolved in the mixed solvent of terepthaloyl moietie and water of step 1); The concentration that makes Lithium Hydroxide MonoHydrate is 0.15 ~ 1.5mol/L, fully stirs, and obtains lithium hydroxide solution;
5) under the state that stirs, the lithium hydroxide solution of step 4) is added drop-wise in the prepared solution that contains phosphoric acid, ferrous sulfate and xitix of step 3), forms and contain sedimentary suspension-s;
6) stir down, polyoxyethylene glycol is added in the suspension-s of step 5), polyoxyethylene glycol quality and prepared target iron lithium phosphate mass percent are 10 ~ 100%; Transfer to then in the autoclave, regulate, make its volume account for reaction kettle inner bag volumetrical 2/3 ~ 4/5 with the mixed solvent that step 1) is prepared; Continue to stir at least 5 minutes, airtight, after being incubated 4 ~ 36 hours under 160 ~ 240 ℃; Reduce to room temperature, take out reaction product, filter; Use deionized water, absolute ethyl alcohol or acetone successively, dry under 40 ℃ ~ 100 ℃ temperature, obtain the iron lithium phosphate monocrystal nano rod.
2. according to the preparation method of the described iron lithium phosphate monocrystal nano rod of claim l, it is characterized in that the purity of said phosphoric acid, six directions ferrous sulfate, Lithium Hydroxide MonoHydrate, xitix, polyoxyethylene glycol, terepthaloyl moietie, absolute ethyl alcohol and acetone all is not less than CP.
3. according to the preparation method of the described iron lithium phosphate monocrystal nano rod of claim l, the radial dimension that it is characterized in that prepared iron lithium phosphate monocrystal nano rod is the 50-200 nanometer, and length is the 0.5-10 micron.
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| WO2015137836A1 (en) * | 2014-03-12 | 2015-09-17 | Akademia Górniczo-Hutnicza im. Stanisława Staszica w Krakowie | Process of fabrication of crystalline nanometric lithium transition metal phosphate |
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| FR3000956A1 (en) * | 2013-01-17 | 2014-07-18 | Commissariat Energie Atomique | PROCESS FOR THE SYNTHESIS OF LIM1-X-Y-ZNYQZFEXPO4 COMPOUND AND ITS USE AS ELECTRODE MATERIAL FOR LITHIUM ACCUMULATOR |
| EP2757068A1 (en) * | 2013-01-17 | 2014-07-23 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | Method for synthesising a LiM1-x-y-zNyQzFexPO4 compound and use thereof as electrode material for a lithium battery |
| JP2017508707A (en) * | 2014-03-12 | 2017-03-30 | アカデミア ゴルニツォ−ハットニツァ アイエム． スタニスラワ スタシツァ ダブリュー クラクフィ | Manufacturing process of nanometer-sized crystalline lithium transition metal phosphate |
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| US10450196B2 (en) | 2014-03-12 | 2019-10-22 | Akademia Górniczo-Hutnicza im. Stanislawa Staszica w Krakowie | Process of fabrication of crystalline nanometric lithium transition metal phosphate |
| CN104183827B (en) * | 2014-08-21 | 2016-08-17 | 浙江大学 | A kind of lithium iron phosphate nano rod and preparation method thereof |
| CN104183827A (en) * | 2014-08-21 | 2014-12-03 | 浙江大学 | Lithium iron phosphate nanorods and preparation method thereof |
| US11076981B2 (en) | 2015-05-30 | 2021-08-03 | Alpha-En Corporation | High purity lithium and associated processes |
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| CN106058247B (en) * | 2016-05-31 | 2018-10-19 | 浙江大学 | Monodisperse lithium iron phosphate nanometer rods and its preparation method and application |
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