CN106340624A - Preparation method of carbon coated LiFePO4 nanorods - Google Patents
Preparation method of carbon coated LiFePO4 nanorods Download PDFInfo
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention discloses a preparation method of carbon coated LiFePO4 nanorods. The preparation method comprises the following steps: adding FeSO4.7H2O, H3PO4, LiOH.H2O, surfactants and ascorbic acid in a beaker filled with distilled water firstly, and transferring to a high-pressure reactor after stirring for a period of time; carrying out a sealed reaction for a period of time, washing after waiting to be naturally cooled, and drying to obtain a precursor A; dissolving carbon sources in distilled water and adding to the precursor A to form a slurry B, ultrasonically stirring the slurry B, and then drying to obtain a mixture C; uniformly grinding the mixture C and then calcining under nitrogen by using a pattern of piecewise calcination, so as to obtain the carbon coated LiFePO4 nanorods. The preparation method disclosed by the invention is simple in process, easy in implementation, and moderate in cost, and further beneficial to shortening of the diffusion path of lithium ions and enhancing of electrode reactions to improve electrochemical properties of anode materials for lithium ion cells.
Description
Technical field
The invention belongs to lithium-ion technology and new material synthesis field are and in particular to a kind of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods
Preparation method.
Background technology
In the last few years, people started increasingly to pay close attention to higher performance and low-cost rechargeable lithium ion batteries in electronics
Application on equipment.Since phosphate of olivine type in 1997 can be as lithium ion anode material by reported first, phosphorus
Sour ferrum lithium (lifepo4) because it is cheap, environmental friendliness, the theoretical specific capacity (170 that nontoxic, cycle performance is good, high
mah g-1) and charge and discharge platform (3.45 v are with respect to li+/ li) the advantages of and be widely studied.But, in lifepo4Crystal
In structure, because the good feo of electric conductivity6Octahedron is by the po of almost insulation4 3-Separate, reduce lifepo4Electric conductivity,
The hexagonal closest packing of oxygen atom three-dimensional limits li+Diffusion.Therefore, low electrical conductivity and the diffusion of slow lithium ion
Limit lifepo4One important parameter of the high rate performance-high-power applications of positive electrode.
Based on this, a lot of researchers are devoted to overcoming these problems in recent years, have done the work of following three aspects: improve
The electrical conductivity (being coated by conductive agent) on surface；Increase lithium ion electrical conductivity (being adulterated by metal cation) and shortening lithium from
The transmission path (by reducing the particle size of material) of son.
Isam etc. is reported in rhombic system, in pnma space group, lithium ion prioritizing selection spreads along b direction of principal axis, and not
It is a axle and the diffusion of c-axis direction, because lithium ion has the migration energy of minimum along the diffusion of b direction of principal axis.Gaberscek etc. adopts
One theoretical model, explains in lifepo4Why ionic conductivity (at room temperature about 10 in crystal-11—10-10s cm-1) than electronic conductivity (at room temperature about 10-9s cm-1) much smaller, the diffusion showing lithium ion is for raising lifepo4
The kinetics aspect of positive electrode is very crucial.Therefore, in order to improve lifepo4The kinetic factor of positive electrode, scholars
Propose a possible approach to pass through to regulate and control lifepo4The micro- knot of positive electrode reaches to shorten size axial along b, this material
Material has very excellent high rate capability because reducing lithium ion the evolving path.Recently, a lot of scholars achieve in this respect
Very big progress.For example, the lifepo of carbon coating is prepared using solvent-thermal method4Stub (is about 50 nm along b direction of principal axis), this material
Material has 155 mah g under 0.1 c discharge-rate-1Specific capacity.Adopt microwave solvent full-boiled process, using tetraethylene glycol (TEG) as solvent system
Standby lifepo4Nanometer rods (are about 25nm along b direction of principal axis), then lifepo are obtained by the cladding of CNT4Nanometer rods/carbon
Nanometer tube composite materials, specific capacity under 0.1c and 10c discharge-rate for this material is respectively 161 and 130 mah g-1.Using
Solvent-thermal method, using ethylene glycol as solvent, Fructus Vitis viniferae acid ferrum, lifepo are replaced with Ferrox.4Material is from diamond shaped (along b axle side
To about 300-500 nm) it is changed into nano-sheet (being about 30 nm along b direction of principal axis).
Additionally, in lifepo4The polarization that material surface coated with conductive agent both can improve electric conductivity and reduce battery, may be used again
Think lifepo4There is provided electron tunnel, for compensating li+Charge balance during deintercalation.Most currently used conductive agent is
Various carbon sources.Using the method for ball milling, by predecomposition at 300 DEG C after reactant stoichiometrically mix homogeneously, Ran Houyu
Conductive black mixing and ball milling, finally sinters at 800 DEG C, obtains the good lifepo of electric conductivity4/c.It is being not added with the condition of white carbon black
Under, lifepo4Specific discharge capacity under the discharge-rate of 1/60 c about 120 mah g-1, under high current density, its capacity is fast
Speed declines；And under conditions of white carbon black exists, with the current discharge of 1/10 c, specific capacity is still up to 120 mah g-1.With
li2co3、fec2o4·2h2O and nh4h2po4For raw material, with molecular weight be 10000 Polyethylene Glycol as carbon source, first ball in the liquid phase
Mill uniformly, is then passed through later stage high-temperature calcination, that is, crystallinity good lifepo is obtained4/ c, it is under 0.06 c discharge-rate
Specific capacity be 162 mah g-1, the specific discharge capacity under 1 c is still up to 139 mah g-1.
Content of the invention
The purpose of the present invention is for above-mentioned present situation, it is desirable to provide a kind of preparation side of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods
Method, the method being conducive to shortening lithium ion the evolving path, strengthening electrode reaction, thus improving the electricity of anode material for lithium-ion batteries
Chemical property.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods
Method, comprises the steps
A), add feso in the beaker fill distilled water4·7h2o、h3po4、lioh∙h2O, surfactant and Vitamin C
Acid, after stirring a period of time, is transferred in autoclave；
B), confined reaction for a period of time, washs after natural cooling, obtains presoma a after being dried；
C), carbon source is dissolved in distilled water, adds presoma a, form serosity b；
D), by serosity b ultrasonic agitation, then it is dried to obtain mixture c；
E), after, grinding uniformly mixture c, the pattern using calcine by steps is calcined under a nitrogen atmosphere, that is, obtain described carbon bag
Cover lithium iron phosphate nano rod.
A kind of preparation method of described carbon-coated LiFePO 4 for lithium ion batteries nanometer rods, its feso4·7h2O consumption is 40 ml distillations
Water 5 30mmol.Its h3po4Consumption is 40 ml distilled water 5 30mmol.Its lioh h2O consumption is 40 ml distilled water 10
120mmol.Its ascorbic acid consumption is 40 ml distilled water 1 15mmol.Its surfactant be dodecylbenzene sodium sulfonate or
Polyethylene Glycol, consumption is 40 ml distilled water 0.1 3mmol.
A kind of preparation method of described carbon-coated LiFePO 4 for lithium ion batteries nanometer rods, in its step b), confined reaction temperature is
120 250 DEG C, the response time be 12 36h, follow-up baking temperature be 50 100 DEG C, drying time be 5 20h.
A kind of preparation method of described carbon-coated LiFePO 4 for lithium ion batteries nanometer rods, in its step c), carbon source is sucrose or Fructus Vitis viniferae
Sugar, the consumption of corresponding 2000mg ferric lithium phosphate precursor a is 100 700mg.
A kind of preparation method of described carbon-coated LiFePO 4 for lithium ion batteries nanometer rods, in its step d), the baking temperature of serosity b is
70 150 DEG C, drying time be 4 18h.
A kind of preparation method of described carbon-coated LiFePO 4 for lithium ion batteries nanometer rods, in its step e) calcine by steps pattern be with
2—7℃ min-1Heating rate 200 400 DEG C calcine 2 8h, then with 15 DEG C of min-1Heating rate exist
400 800 DEG C of calcining 7 12h.
The invention has the beneficial effects as follows: preparation method process is simple of the present invention, it is easily achieved, and moderate cost, in addition
Preparation method of the present invention also helping shortening lithium ion the evolving path, strengthening electrode reaction, thus improving lithium ion cell positive
The chemical property of material.
Brief description
Fig. 1 is the stereoscan photograph of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods in the embodiment of the present invention 1；
Fig. 2 is the transmission electron microscope photo of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods in the embodiment of the present invention 1；
Fig. 3 is charging and discharging curve under 0.1 10c electric current density for the carbon-coated LiFePO 4 for lithium ion batteries nanometer rods in the embodiment of the present invention 1
(voltage range is 2.5 4.2v, defines 1c=170mag-1).
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is described in further detail.
Referring to figs. 1 to shown in Fig. 3, the present invention adopts hydro-thermal reaction, prepares ferric phosphate lithium ion electricity with surfactant
Pond positive electrode, obtains along the controlled nanometer rods of b direction of principal axis size, the specific discharge capacity of LiFePO4 and high rate performance are with material
Material improves in the reduction of b direction of principal axis size, and the area shortening it in the axial size of b and increase (010) face is conducive to contracting
Short lithium ion the evolving path, enhancing electrode reaction, thus improve the chemical property of carbon-coated lithium iron phosphate composite.
Embodiment 1:
A) 15 mmol feso are added in the beaker filling 40 ml distilled water4·7h2o、15 mmol h3po4、45 mmol
lioh∙h2O, 0.6 mmol dodecylbenzene sodium sulfonate and 7.5 mmol ascorbic acid, after stirring 20 min, are transferred to high pressure anti-
Answer in kettle；
B) confined reaction 24h at 170 DEG C, washs after natural cooling, 12h is dried, obtains presoma a at 60 DEG C；
C) 200mg sucrose is dissolved in 4ml distilled water, adds 2000mg presoma a, form serosity b；
D) by after serosity b ultrasonic agitation 15 min, 12h is dried at 90 DEG C and obtains mixture；
E), after said mixture c being ground uniformly, calcine under a nitrogen atmosphere.Using the pattern of calcine by steps, with 4 DEG C of min-1
Heating rate 350 DEG C calcine 4h, then with 2 DEG C of min-1Heating rate 650 DEG C calcine 9h, that is, obtain described carbon bag
Cover lithium iron phosphate nano rod.
Embodiment 2:
A) 30 mmol feso are added in the beaker filling 40 ml distilled water4·7h2o、30 mmol h3po4、90 mmol
lioh∙h2O, 1.5 mmol Polyethylene Glycol and 15 mmol ascorbic acid, after stirring 20 min, are transferred in autoclave；
B) confined reaction 36 h at 220 DEG C, washs after natural cooling, 15 h is dried, obtains presoma a at 80 DEG C；
C) 450 mg sucrose are dissolved in 4ml distilled water, add 2000 mg presoma a, form serosity b；
D) obtain mixture by 8 h after serosity b ultrasonic agitation 15 min, are dried at 120 DEG C；
E), after said mixture c being ground uniformly, calcine under a nitrogen atmosphere, using the pattern of calcine by steps, with 3 DEG C of min-1
Heating rate 400 DEG C calcine 7 h, then with 5 DEG C of min-1Heating rate 800 DEG C calcine 5 h, that is, obtain described carbon
Coated LiFePO 4 for lithium ion batteries nanometer rods.
Embodiment 3:
A) 5 mmol feso are added in the beaker filling 40 ml distilled water4·7h2o、5 mmol h3po4、10 mmol
lioh∙h2O, 0.1 mmol dodecylbenzene sodium sulfonate and 1 mmol ascorbic acid, after stirring 20 min, are transferred to reaction under high pressure
In kettle；
B) confined reaction 12h at 120 DEG C, washs after natural cooling, 20h is dried, obtains presoma a at 50 DEG C；
C) 100mg glucose is dissolved in 4ml distilled water, adds 2000mg presoma a, form serosity b；
D) by after serosity b ultrasonic agitation 15 min, 18h is dried at 70 DEG C and obtains mixture；
E), after said mixture c being ground uniformly, calcine under a nitrogen atmosphere.Using the pattern of calcine by steps, with 2 DEG C of min-1
Heating rate 200 DEG C calcine 8h, then with 1 DEG C of min-1Heating rate 400 DEG C calcine 7h, that is, obtain described carbon bag
Cover lithium iron phosphate nano rod.
Embodiment 4:
A) 5 mmol feso are added in the beaker filling 40 ml distilled water4·7h2o、5 mmol h3po4、120 mmol
lioh∙h2O, 3 mmol Polyethylene Glycol and 1 mmol ascorbic acid, after stirring 20 min, are transferred in autoclave；
B) confined reaction 36h at 250 DEG C, washs after natural cooling, 50h is dried, obtains presoma a at 100 DEG C；
C) 700mg glucose is dissolved in 4ml distilled water, adds 2000mg presoma a, form serosity b；
D) by after serosity b ultrasonic agitation 15 min, 4h is dried at 150 DEG C and obtains mixture；
E), after said mixture c being ground uniformly, calcine under a nitrogen atmosphere.Using the pattern of calcine by steps, with 7 DEG C of min-1
Heating rate 200 DEG C calcine 2h, then with 1 DEG C of min-1Heating rate 400 DEG C calcine 12h, that is, obtain described carbon bag
Cover lithium iron phosphate nano rod.
Above-described embodiment only principle of the illustrative present invention and its effect, and the embodiment that part is used, for
For those of ordinary skill in the art, without departing from the concept of the premise of the invention, can also make some deformation and
Improve, these broadly fall into protection scope of the present invention.
Claims (10)
1. a kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods it is characterised in that: comprise the steps
A), add feso in the beaker fill distilled water4·7h2o、h3po4、lioh∙h2O, surfactant and ascorbic acid,
After stirring a period of time, it is transferred in autoclave；
B), confined reaction for a period of time, washs after natural cooling, obtains presoma a after being dried；
C), carbon source is dissolved in distilled water, adds presoma a, form serosity b；
D), by serosity b ultrasonic agitation, then it is dried to obtain mixture c；
E), after, grinding uniformly mixture c, the pattern using calcine by steps is calcined under a nitrogen atmosphere, that is, obtain described carbon bag
Cover lithium iron phosphate nano rod.
2. a kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods according to claim 1 is it is characterised in that described
feso4·7h2O consumption is 40 ml distilled water 5 30mmol.
3. a kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods according to claim 1 is it is characterised in that described
h3po4Consumption is 40 ml distilled water 5 30mmol.
4. a kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods according to claim 1 is it is characterised in that described
lioh∙h2O consumption is 40 ml distilled water 10 120mmol.
5. a kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods according to claim 1 is it is characterised in that described
Ascorbic acid consumption is 40 ml distilled water 1 15mmol.
6. a kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods according to claim 1 is it is characterised in that described
Surfactant is dodecylbenzene sodium sulfonate or Polyethylene Glycol, and consumption is 40 ml distilled water 0.1 3mmol.
7. a kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods according to claim 1 is it is characterised in that described
In step b) confined reaction temperature be 120 250 DEG C, the response time be 12 36h, follow-up baking temperature is 50 100 DEG C, dry
The dry time is 5 20h.
8. a kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods according to claim 1 is it is characterised in that described
In step c), carbon source is sucrose or glucose, and the consumption of corresponding 2000mg ferric lithium phosphate precursor a is 100 700mg.
9. a kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods according to claim 1 is it is characterised in that described
In step d) the baking temperature of serosity b be 70 150 DEG C, drying time be 4 18h.
10. a kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries nanometer rods according to claim 1 is it is characterised in that described
Step e) in calcine by steps pattern be with 27 DEG C of min-1Heating rate 200 400 DEG C calcine 2 8h, then with
1—5℃ min-1Heating rate 400 800 DEG C calcine 7 12h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106908502A (en) * | 2017-03-27 | 2017-06-30 | 电子科技大学 | The preparation method of the glucose sensor enzyme electrode of carbon-coated magnetic ferrite modification |
| CN107623107A (en) * | 2017-10-16 | 2018-01-23 | 中南大学 | A kind of method for preparing lithium manganese phosphate cell positive material |
| CN108155368A (en) * | 2017-12-29 | 2018-06-12 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七二研究所） | A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods |
| CN109037658A (en) * | 2018-08-31 | 2018-12-18 | 重庆工商大学 | A kind of lithium iron phosphate positive material preparation method of polymer overmold |
| CN109904409A (en) * | 2019-01-14 | 2019-06-18 | 广东工业大学 | A kind of lithium iron phosphate nano stick/graphene composite material and its preparation method and application |
| CN114380308A (en) * | 2021-08-20 | 2022-04-22 | 山东瑞福锂业有限公司 | Preparation process and method of lithium carbonate nanowire with excellent energy storage performance for lithium ion battery |
| CN114613945A (en) * | 2022-04-02 | 2022-06-10 | 北京师范大学 | Preparation method of lithium ion battery anode |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106908502A (en) * | 2017-03-27 | 2017-06-30 | 电子科技大学 | The preparation method of the glucose sensor enzyme electrode of carbon-coated magnetic ferrite modification |
| CN107623107A (en) * | 2017-10-16 | 2018-01-23 | 中南大学 | A kind of method for preparing lithium manganese phosphate cell positive material |
| CN108155368A (en) * | 2017-12-29 | 2018-06-12 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七二研究所） | A kind of preparation method of carbon coating lithium manganese phosphate nanometer rods |
| CN109037658A (en) * | 2018-08-31 | 2018-12-18 | 重庆工商大学 | A kind of lithium iron phosphate positive material preparation method of polymer overmold |
| CN109904409A (en) * | 2019-01-14 | 2019-06-18 | 广东工业大学 | A kind of lithium iron phosphate nano stick/graphene composite material and its preparation method and application |
| CN114380308A (en) * | 2021-08-20 | 2022-04-22 | 山东瑞福锂业有限公司 | Preparation process and method of lithium carbonate nanowire with excellent energy storage performance for lithium ion battery |
| CN114380308B (en) * | 2021-08-20 | 2023-12-08 | 山东瑞福锂业有限公司 | Preparation process and method of lithium carbonate nanowire with excellent energy storage performance for lithium ion battery |
| CN114613945A (en) * | 2022-04-02 | 2022-06-10 | 北京师范大学 | Preparation method of lithium ion battery anode |
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