CN102530905A - Preparation method of nano FePO4 with controllable particle size - Google Patents
Preparation method of nano FePO4 with controllable particle size Download PDFInfo
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- CN102530905A CN102530905A CN2011104457972A CN201110445797A CN102530905A CN 102530905 A CN102530905 A CN 102530905A CN 2011104457972 A CN2011104457972 A CN 2011104457972A CN 201110445797 A CN201110445797 A CN 201110445797A CN 102530905 A CN102530905 A CN 102530905A
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Abstract
The method provides a method for preparing nano FePO4. The method comprises the steps of: a. dissolving soluble phosphorus source and soluble ferric iron salt in deionized water, and adjusting the pH value with an acid until the solution is clear and transparent; b. adding an organic solvent and a surfactant to the solution obtained in the step a, and stirring until the solution is in a homogeneous, clear and stable state; c. adjusting the solution obtained in the step b to a certain temperature, placing the solution in an ultrasonic field, slowly adding an alkaline solution under vigorously stirring, and adjusting the solution to a certain pH value to obtain FePO4 colloidal particle sol; and d. centrifugally cleaning the FePO4 colloidal particle sol with deionized water three times, ultrasonically dispersing in an organic solvent, and drying in a vacuum drying oven at a certain drying temperature for a certain drying time to obtain nano FePO4. The method for preparing FePO4 provided by the invention has the characteristics of simple production process and low cost; and the product obtained by the method has low impurity content, excellent appearance and controllable particle size.
Description
Technical field
The present invention relates to field of materials, particularly, the present invention relates to nanometer Fe PO
4The preparation method.
Background technology
Before the lithium ion secondary battery anode material ferric lithium phosphate invention, tertiary iron phosphate is mainly used in fields such as ceramic foodstuff additive, also is used as support of the catalyst in recent years.Flourish along with lithium ion battery anode material lithium iron phosphate, tertiary iron phosphate also is widely used in the presoma of preparation high-performance iron phosphate lithium positive electrode material.
In recent years, serious day by day along with the progressively exhausted and vehicle exhaust environmental pollution of whole world petroleum resources, power truck (EV) or hybrid electric vehicle (HEV) and corresponding electrical source of power are developed rapidly.Plurality of advantages such as the lithium ion battery volume is little, WV is high, memory-less effect, pollution are little, have extended cycle life, thereby receive extensive welcome.Anode material for lithium-ion batteries is a key factor of decision battery performance, and business-like at present positive electrode material has LiCoO
2, LiNiO
2, LiMn
2O
4Deng, but other positive electrode material of comparing, LiFePO
4Have two significant advantages: excellent security can and be followed the voltinism ability, and this is because its inner unique scaffolding structure makes its molecular structure in working cycle highly stable, therefore generally believes LiFePO in recent years in the world
4It is the best novel anode material of high-energy power battery.
Although LiFePO
4Have numerous advantages, but the some shortcomings part is also arranged, particularly present LiFePO
4Main application fields is a power lithium-ion rechargeable battery, so make these shortcomings seem more outstanding during heavy-current discharge: at first, its specific conductivity is low, pure LiFePO
4Specific conductivity generally in this one magnitude of 10-10S/m, this problem is seriously restricting its practical application as high-power battery; Secondly, because of LiFePO
4Structure is that the passage that provides of lithium ion diffusion is limited, and lithium ion is in the inner embedding of crystal grain and to deviate from speed slow, and this causes working as LiFePO
4The embedding of lithium ion and deviate from speed when being used for high-multiplying power discharge less than the interface chemistry pace of change, gram volume is lower and polarization is severe when showing as high-multiplying power discharge; At last, its tap density and compacted density are low causes the energy density of battery low; Granule-morphology is difficult to control and causes its processing characteristics relatively poor.These problems cause it on commercial applications, to have a lot of obstacles, so must solve LiFePO from material prepn
4These difficulties that faced.At many raising LiFePO
4In the method for performance, obtain the LiFePO of nanometer
4Thereby reduce the diffusion length of Li+ in crystal grain, help to improve greatly LiFePO
4High magnification impulse electricity performance.
Synthetic LiFePO
4Scheme a lot, in many synthetic schemess, with FePO
4Be the synthetic LiFePO of presoma
4Has salient feature: FePO
4With LiFePO
4Have similar crystalline structure, and Li+ at high temperature has fabulous diffusion, so can be through control FePO
4Granule-morphology, size and size-grade distribution synthesize ideal nanometer LiFePO
4, also be FePO
4Hereditary property.In view of the above, we can relatively easily utilize various soft chemical methods to prepare nanometer Fe PO
4, synthesize the controllable nano FePO of particle diameter, pattern, size-grade distribution through control pH value, temperature, concentration, tensio-active agent and other condition
4, and through the synthetic LiFePO of high temperature solid state reaction
4, simultaneously with FePO
4Particle size, pattern etc. entail LiFePO
4And the LiFePO of suitable particles pattern, size, size-grade distribution
4Be to have excellent electrochemical character lithium ion battery essential condition.
Therefore, synthesize the controllable nano FePO of particle diameter, pattern, size-grade distribution through control pH value, temperature, concentration, tensio-active agent and other condition
4Thereby, utilize this controllable nano FePO
4Be the synthetic LiFePO of presoma
4Method be very significant.
Summary of the invention
The invention provides synthesis of nano FePO
4Method.
According to an aspect of the present invention, a kind of preparation nanometer Fe PO is provided
4Method, may further comprise the steps:
A. soluble sources and solubility trivalent iron salt are dissolved in the deionized water, utilize acid to regulate its pH value and make solution be in clear;
B. in a step gained solution, add organic solvent, tensio-active agent and be stirred to solution evenly, clarification, steady state;
C. regulate b step gained solution to certain temperature, insert solution in the ultrasonic field then, and under vigorous stirring, slowly add basic soln, regulator solution to certain pH value obtains FePO
4Micelle colloidal sol;
D. with deionized water to said FePO
4Micelle colloidal sol carries out eccentric cleaning three times, and ultra-sonic dispersion is in organic solvent, and it is dry to put into vacuum drying oven, and dry certain hour obtains having the greyish white or light yellow ball shaped nano FePO of better dispersiveness under certain drying temperature
4
In aforesaid method, wherein said method is included in and adds the pattern adjusting control agent among the step b.
In aforesaid method, wherein said soluble sources is selected from phosphoric acid, sodium phosphate, potassiumphosphate, ammonium phosphate, disodium-hydrogen, potassium phosphate,monobasic, ammonium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate or primary ammonium phosphate.
In aforesaid method, wherein said trivalent iron salt is iron nitrate, iron(ic)chloride or ferric sulfate.
In aforesaid method, the concentration of wherein said soluble sources or molysite is all in 0.05mol/L to 4mol/L scope.
In aforesaid method, wherein said acid is sulfuric acid, nitric acid or hydrochloric acid.
In aforesaid method, wherein the organic solvent among the step b is selected from ethanol, terepthaloyl moietie, Virahol, USP Kosher, lauryl alcohol, glycol ether, triglycol, Tetraglycol 99, PEG 400, one or more in the trihydroxybutane.
In aforesaid method, wherein among the step b volume of organic solvent in 0% to 30% scope.
In aforesaid method, wherein said tensio-active agent is selected from one or more in sodium lauryl sulphate, cetyl trimethylammonium bromide, polyoxyethylene glycol, Z 150PH, T 46155 octyl phenolic ether, the octyl phenyl Soxylat A 25-7.
In aforesaid method, wherein said pattern adjusting control agent is selected from one or more in Isopropylamine, diethylamine, hexanediamine, triethylamine, quadrol, Diisopropylamine, diethylolamine, diethylenetriamine, the triethylene tetramine.
In aforesaid method, the add-on of wherein said pattern adjusting control agent is the 0-2% of liquor capacity.
In aforesaid method, the add-on of wherein said tensio-active agent is the 0-3% of solution quality.
In aforesaid method, wherein said basic soln is selected from one or more of soluble carbon hydrochlorate, ammoniacal liquor or organic amine.
In aforesaid method, wherein said soluble carbon hydrochlorate is selected from yellow soda ash, sodium hydrogencarbonate, salt of wormwood, saleratus, volatile salt or bicarbonate of ammonia.
In aforesaid method, the concentration of wherein said basic soln is in the scope of 0.1mol/L to 6mol/L.
In aforesaid method, wherein the temperature among the step c is between-5 to 20 ℃.
In aforesaid method, the frequency of wherein said ultrasonic field is between 10K to 100KHz, and power is between 0 to 3000W.
In aforesaid method, wherein the pH value among the step c is between 1.0 to 4.5.
In aforesaid method, wherein the organic solvent in the steps d is selected from propyl alcohol, butanols, terepthaloyl moietie, acetone, Virahol, USP Kosher, methyl-sulphoxide, N, one or more in dinethylformamide, the N-Methyl pyrrolidone.
In aforesaid method, wherein the organic solvent in the steps d is propyl alcohol, butanols, terepthaloyl moietie, acetone, Virahol, USP Kosher, methyl-sulphoxide, N, one or more in dinethylformamide, the N-Methyl pyrrolidone and ethanol mixed solvent.
In aforesaid method, wherein said drying temperature is between 100 to 120 ℃.
In aforesaid method, wherein said time of drying is between 0.5 to 10 hour.
Use the prepared nano ferric phosphate of method of the present invention to have the following advantages:
Production technique is simple, cost is low;
Compare with regulate pH value with strong base solutions such as NaOH, with carbonate adjusting pH value, then reacting phase is to Fe (OH) in gentleness and the product
3, Fe
2O
3Impurity is few;
Regulate the pattern of controlling product with organism such as polyvalent alcohol and organic amines, products obtained therefrom has good shapes;
Originally be reflected under the low relatively temperature and react, and consider soltion viscosity, ultrasonic field effect, reaction multiple factors such as the bubble that generates, through various reaction conditions control grain diameters;
The pattern of nano ferric phosphate and particle size have the advantages that arbitrarily to regulate and control, and particle diameter can change between 10nm～300nm.
Description of drawings
Fig. 1 illustrates the X-ray diffractogram (XRD figure) of the nano ferric phosphate of embodiment 6 preparations.
Fig. 2 illustrates the transmission electron microscope picture (TEM figure) of embodiment 6 preparation nano ferric phosphates.
Fig. 3 illustrates the scanning electron microscope diagram (SEM figure) of embodiment 6 preparation nano ferric phosphates.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail, but these embodiment are not used in qualification the present invention.
Embodiment 1
The phosphoric acid and being dissolved in the 100ml deionized water of each 0.01mol of iron nitrate that will meet stoichiometric ratio are made into settled solution; Add each 1g surface active agent polyvinyl alcohol and PEG1000 to solution; And add organic solvent terepthaloyl moietie 10ml and pattern adjusting control agent quadrol 1ml, and be stirred to solution evenly, clarification, steady state.This mixed settled solution temperature is transferred to 0 ℃, and the back is inserted solution in certain ultrasonic field that (10KHz 1000W), slowly joins the sodium carbonate solution of 2mol/L in the above-mentioned settled solution simultaneously, and the pH value of solution value is adjusted to 1.5, necessarily obtains FePO under vigorous stirring
4Micelle colloidal sol.Gained colloidal sol is carried out centrifugation; And use the deionized water ultrasonic cleaning; Repeatedly after three times with gained tertiary iron phosphate ultra-sonic dispersion in n-propyl alcohol; After put into vacuum drying oven and under the certain vacuum degree, carry out drying, at certain 105 ℃ down after dry 5 hours, the greyish white or light yellow ball shaped nano tertiary iron phosphate (FePO that obtains having better dispersiveness
4H
2O).(gained FePO
4.H
2The XRD of O, TEM, SEM see accompanying drawing 1, accompanying drawing 2, accompanying drawing 3 respectively)
Embodiment 2
0.4mol primary ammonium phosphate and 0.4mol iron(ic)chloride is dissolved in the 100ml deionized water is made into settled solution; Add each 3g surface active agent polyvinyl alcohol to solution; And add organic solvent 20ml USP Kosher and pattern adjusting control agent diethylenetriamine 1ml, and be stirred to solution evenly, clarification, steady state.This mixed settled solution temperature is transferred to 15 ℃; The back is inserted solution in certain ultrasonic field that (80KHz 2000W), slowly joins the sodium carbonate solution of 6mol/L in the above-mentioned settled solution simultaneously under vigorous stirring; The pH value of solution value is adjusted to 4.0, necessarily obtains FePO
4Micelle colloidal sol.Gained colloidal sol is carried out centrifugation; And use the deionized water ultrasonic cleaning; Repeatedly after three times with gained tertiary iron phosphate ultra-sonic dispersion in propyl carbinol; After put into vacuum drying oven and under the certain vacuum degree, carry out drying, at certain 110 ℃ down after dry 8 hours, the greyish white or light yellow ball shaped nano tertiary iron phosphate (FePO that obtains having better dispersiveness
4H
2O).
Embodiment 3
0.05mol sodium phosphate and 0.05mol iron nitrate are dissolved in the 100ml deionized water; Utilize nitric acid to regulate its pH value; Be made into the settled solution of 0.5mol/L; Add each 3% surfactant emulsifiers OP-10 and Macrogol 4000 to solution, and add organic solvent triglycol (30%) and pattern adjusting control agent diethylolamine 1%, and be stirred to solution evenly, clarification, steady state.Sodium carbonate solution with 6mol/L under vigorous stirring slowly joins in the above-mentioned settled solution, and the pH value of solution value is adjusted to 4.5, obtains FePO
4Micelle colloidal sol.Gained colloidal sol is carried out centrifugation; And use the deionized water ultrasonic cleaning; Repeatedly after three times with gained tertiary iron phosphate ultra-sonic dispersion in the mixed solvent of ethanol and terepthaloyl moietie; After put into vacuum drying oven and under the certain vacuum degree, carry out drying, at certain 120 ℃ down after dry 10 hours, the greyish white or light yellow ball shaped nano tertiary iron phosphate (FePO that obtains having better dispersiveness
4H
2O).
Embodiment 4
0.1mol SODIUM PHOSPHATE, MONOBASIC and 0.1mol iron nitrate are dissolved in the 100ml deionized water, are made into settled solution, and add organic solvent 10ml USP Kosher and 15ml glycol ether and pattern adjusting control agent hexanediamine 0.5ml, and be stirred to that solution is even, clarification, steady state.This mixed settled solution temperature is transferred to 20 ℃; The back is inserted solution in certain ultrasonic field that (50KHz 500W), mixes the saleratus of 1mol/L with basic soln with ammoniacal liquor simultaneously and slowly joins in the above-mentioned settled solution under vigorous stirring; The pH value of solution value is adjusted to 1.0, obtains FePO
4Micelle colloidal sol.Gained colloidal sol is carried out centrifugation; And use the deionized water ultrasonic cleaning; Repeatedly after three times with gained tertiary iron phosphate ultra-sonic dispersion in the mixed solvent of ethanol and terepthaloyl moietie; After put into vacuum drying oven and under the certain vacuum degree, carry out drying, at certain 100 ℃ down after dry 3 hours, the greyish white or light yellow ball shaped nano tertiary iron phosphate (FePO that obtains having better dispersiveness
4H
2O).
Embodiment 5
0.005mol sodium phosphate and 0.005mol iron nitrate are dissolved in the 100ml deionized water; Utilize nitric acid to regulate its pH value; Be made into the settled solution of 0.05mol/L; To solution add each 0.5g tensio-active agent sodium lauryl sulphate and and PEG20000, and add pattern adjusting control agent diethylolamine 1ml, and be stirred to solution evenly, clarification, steady state.This mixed settled solution temperature is transferred to-5 ℃; The back is inserted solution in certain ultrasonic field that (10KHz 3000W), slowly joins the sodium carbonate solution of 2mol/L in the above-mentioned settled solution simultaneously under vigorous stirring; The pH value of solution value is adjusted to 2.5, necessarily obtains FePO
4Micelle colloidal sol.Gained colloidal sol is carried out centrifugation; And use the deionized water ultrasonic cleaning; Repeatedly after three times with gained tertiary iron phosphate ultra-sonic dispersion in the mixed solvent of ethanol and terepthaloyl moietie; After put into vacuum drying oven and under the certain vacuum degree, carry out drying, at certain 100 ℃ down after dry 10 hours, the greyish white or light yellow ball shaped nano tertiary iron phosphate (FePO that obtains having better dispersiveness
4H
2O).
Embodiment 6
Potassium primary phosphate and the 0.0.01mol iron nitrate of 0.0.01mol are dissolved in the 100ml ionized water; Be made into settled solution; Add each 1g surfactant emulsifiers OP-10 and Macrogol 4000 to solution, and add the 15ml triglycol, and be stirred to solution evenly, clarification, steady state.This mixed settled solution temperature is transferred to 10 ℃; The back is inserted solution in certain ultrasonic field that (100KHz 1000W), slowly joins the ammonium bicarbonate soln of 3mol/L in the above-mentioned settled solution simultaneously under vigorous stirring; The pH value of solution value is adjusted to 2.5, necessarily obtains FePO
4Micelle colloidal sol.Gained colloidal sol is carried out centrifugation; And use the deionized water ultrasonic cleaning; Repeatedly after three times with gained tertiary iron phosphate ultra-sonic dispersion in the USP Kosher solvent; After put into vacuum drying oven and under the certain vacuum degree, carry out drying, at certain 120 ℃ down after dry 0.5 hour, the greyish white or light yellow ball shaped nano tertiary iron phosphate (FePO that obtains having better dispersiveness
4H
2O).
Though described the present invention with reference to specific embodiments of the present invention, those skilled in the art is to be understood that and under the situation that does not break away from true spirit of the present invention and scope, can carries out various changes and can replace equivalents.In addition, many modifications can be carried out so that particular case, material, material composition, method, method steps adapt to the spirit and scope of the present invention.All these changes will be in the scope of subsidiary claims.
Claims (22)
1. one kind prepares nanometer Fe PO
4Method, comprising:
A. soluble sources and solubility trivalent iron salt are dissolved in the deionized water, utilize acid to regulate its pH value and make solution be in clear;
B. in a step gained solution, add organic solvent, tensio-active agent and be stirred to solution evenly, clarification, steady state;
C. regulate b step gained solution to certain temperature, insert solution in the ultrasonic field then, and under vigorous stirring, slowly add basic soln, regulator solution to certain pH value obtains FePO
4Micelle colloidal sol;
D. with deionized water to said FePO
4Micelle colloidal sol carries out eccentric cleaning three times, and ultra-sonic dispersion is in organic solvent, and it is dry to put into vacuum drying oven, and dry certain hour obtains nanometer Fe PO under certain drying temperature
4
2. method according to claim 1, wherein said method are included in and add the pattern adjusting control agent among the step b.
3. method according to claim 1, wherein said soluble sources is selected from phosphoric acid, sodium phosphate, potassiumphosphate, ammonium phosphate, disodium-hydrogen, potassium phosphate,monobasic, ammonium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium primary phosphate or primary ammonium phosphate.
4. method according to claim 1, wherein said trivalent iron salt are iron nitrate, iron(ic)chloride or ferric sulfate.
5. method according to claim 1, the concentration of wherein said soluble sources or molysite are all in 0.0.1mol/L to 4mol/L scope.
6. method according to claim 1, wherein said acid are sulfuric acid, nitric acid or hydrochloric acid.
7. method according to claim 1, wherein the organic solvent among the step b is selected from ethanol, terepthaloyl moietie, Virahol, USP Kosher, lauryl alcohol, glycol ether, triglycol, Tetraglycol 99, PEG 400, one or more in the trihydroxybutane.
8. method according to claim 1, wherein among the step b volume of organic solvent in 0% to 30% scope.
9. method according to claim 1, wherein said tensio-active agent are selected from one or more in sodium lauryl sulphate, cetyl trimethylammonium bromide, polyoxyethylene glycol, Z 150PH, T 46155 octyl phenolic ether, the octyl phenyl Soxylat A 25-7.
10. method according to claim 1, wherein said pattern adjusting control agent is selected from one or more in Isopropylamine, diethylamine, hexanediamine, triethylamine, quadrol, Diisopropylamine, diethylolamine, diethylenetriamine, the triethylene tetramine.
11. method according to claim 1, the add-on of wherein said pattern adjusting control agent are the 0-2% of liquor capacity.
12. method according to claim 1, the add-on of wherein said tensio-active agent are the 0-3% of solution quality.
13. method according to claim 1, wherein said basic soln is selected from one or more of soluble carbon hydrochlorate, ammoniacal liquor or organic amine.
14. method according to claim 12, wherein said soluble carbon hydrochlorate is selected from yellow soda ash, sodium hydrogencarbonate, salt of wormwood, saleratus, volatile salt or bicarbonate of ammonia.
15. method according to claim 1, the concentration of wherein said basic soln is in the scope of 0.1mol/L to 6mol/L.
16. method according to claim 1, wherein the temperature among the step c is between-5 to 20 ℃.
17. method according to claim 1, the frequency of wherein said ultrasonic field are between 10K to 100KHz, power is between 0 to 3000W.
18. method according to claim 1, wherein the pH value among the step c is between 1.0 to 4.5.
19. method according to claim 1, wherein the organic solvent in the steps d is selected from propyl alcohol, butanols, terepthaloyl moietie, acetone, Virahol, USP Kosher, methyl-sulphoxide, N, one or more in dinethylformamide, the N-Methyl pyrrolidone.
20. method according to claim 1; Wherein the organic solvent in the steps d is propyl alcohol, butanols, terepthaloyl moietie, acetone, Virahol, USP Kosher, methyl-sulphoxide, N, one or more in dinethylformamide, the N-Methyl pyrrolidone and ethanol mixed solvent.
21. method according to claim 1, wherein said drying temperature is between 100 to 120 ℃.
22. method according to claim 1, wherein said time of drying is between 0.5 to 10 hour.
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| CN104505495A (en) * | 2014-12-09 | 2015-04-08 | 山东精工电子科技有限公司 | Method for ultrasonic preparation of nano iron phosphate of lithium iron phosphate |
| CN104619634A (en) * | 2012-08-10 | 2015-05-13 | 三星精密化学株式会社 | Method for preparing nano-sized iron phosphate particles |
| CN105118995A (en) * | 2015-10-14 | 2015-12-02 | 湖南省正源储能材料与器件研究所 | Production method of battery-grade iron phosphate |
| CN105645371A (en) * | 2016-01-08 | 2016-06-08 | 西南大学 | One-step preparation method and application of nano transition metal phosphates |
| CN108793116A (en) * | 2018-06-27 | 2018-11-13 | 内江师范学院 | The preparation method and applications of different-shape micron ferric phosphate |
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| CN108793116A (en) * | 2018-06-27 | 2018-11-13 | 内江师范学院 | The preparation method and applications of different-shape micron ferric phosphate |
| CN108840317A (en) * | 2018-09-28 | 2018-11-20 | 广东光华科技股份有限公司 | A kind of preparation method of high-purity high-pressure solid battery-grade iron phosphate |
| CN110010890A (en) * | 2018-12-26 | 2019-07-12 | 广西大学 | A kind of normal-temperature reaction preparation method of ball shaped nano ferric phosphate |
| CN110482512A (en) * | 2019-07-12 | 2019-11-22 | 乳源东阳光磁性材料有限公司 | A kind of preparation method of battery-grade iron phosphate |
| CN111653846A (en) * | 2020-07-27 | 2020-09-11 | 中南大学 | Treatment method of waste lithium iron phosphate battery |
| CN112436132A (en) * | 2020-12-10 | 2021-03-02 | 桂林理工大学 | Method for preparing in-situ carbon-coated porous ferric phosphate material by adopting sweet osmanthus |
| CN112436132B (en) * | 2020-12-10 | 2021-07-02 | 桂林理工大学 | Method for preparing in-situ carbon-coated porous ferric phosphate material by adopting sweet osmanthus |
| CN112978696A (en) * | 2021-02-23 | 2021-06-18 | 长沙学院 | Iron phosphate and preparation method and application thereof |
| CN116143099A (en) * | 2023-02-24 | 2023-05-23 | 南京理工大学 | Method for cooperatively synthesizing lithium iron phosphate electrode material by using ethylene glycol and sodium dodecyl sulfate |
| CN116143099B (en) * | 2023-02-24 | 2024-03-19 | 南京理工大学 | Method for cooperatively synthesizing lithium iron phosphate electrode material by using ethylene glycol and sodium dodecyl sulfate |
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