CN110364694A - A kind of preparation method of composite ferric lithium phosphate material - Google Patents
A kind of preparation method of composite ferric lithium phosphate material Download PDFInfo
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- CN110364694A CN110364694A CN201810319076.9A CN201810319076A CN110364694A CN 110364694 A CN110364694 A CN 110364694A CN 201810319076 A CN201810319076 A CN 201810319076A CN 110364694 A CN110364694 A CN 110364694A
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- H01M4/00—Electrodes
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- H—ELECTRICITY
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Abstract
A kind of preparation method of composite ferric lithium phosphate material, first, the metal nanometer line of high length-diameter ratio is prepared using a kind of solvent-thermal method, then the metal nanometer line prepared is uniformly mixed with lithium iron phosphate precursor solution, after the stirring of certain time, obtained mixed solution is transferred in microwave reactor and is reacted, after 5-30 minutes, stop microwave reaction, after product cooled to room temperature, it is handled by centrifuge washing, obtain the one-dimensional composite ferric lithium phosphate material original powder of LiFePO4 cladding metal nanometer line, later, the LiFePO4 original powder is placed in microwave reactor and is sintered, and finally obtain product composite ferric lithium phosphate material.
Description
Technical field
The present invention relates to the field of chemical synthesis, and in particular to a kind of preparation method of novel phosphoric acid iron lithium composite material.
Background technique
Lithium ion battery is as a kind of secondary cell, either in electronic information or energy traffic or industrial production
And be all widely used in daily life, currently, with the New energy electric of clean energy resource electric energy substitution conventional fossil fuel
Automobile is more prevalent, and the key technology of Development of Electric Vehicles is that the excavation of power battery potentiality, lithium ion battery due to
With cell voltage is high, energy density is big, specific capacity is big, have extended cycle life, self-discharge rate is low and the advantages such as memory-less effect
And obtain the approval of industry.
Since nineteen ninety, Sony successfully obtained lithium ion battery for the first time, in recent years, about lithium ion battery
Research is advanced by leaps and bounds, and the positive material of the lithium ion battery used for the first time is cobalt acid lithium, and negative electrode material is ungraphitised carbon, it
Afterwards, people have carried out great expansion for the classification of positive electrode and negative electrode material.Currently, with J.Goodenough et al.
It was found that olivine-type LiFePO4 be the anode material for lithium-ion batteries of representative and the negative electrode material using carbon material as representative is
Main battery electrode material, since LiFePO4 has preferable charge-discharge performance, people conduct in-depth research it,
Not only include the expansion of preparation method, further includes the synthesis of various different-shapes.
Wherein, Chinese patent CN 102104149A discloses the iron lithium phosphate compound anode material in a kind of lithium ion battery
Material and preparation method thereof, author will use containing lithium, iron content, phosphorous raw material presoma, through ball milling, drying, mistake in the invention
It after sieve, pre-burning, calcining, is uniformly mixed with nano wire, then the compound iron lithium phosphate compound anode material of nano wire is made by annealing
Material, the combination electrode material prepared by this method is conductive excellent, to improve the reversible capacity of battery, forthright again
Energy and cycle life.In addition, GuoxiuWang of Canadian University of Wollongong et al. is in 2008 in " Journal of Power
Sources " on one-dimensional lithium iron phosphate nano line is prepared by the method for hydro-thermal in the article delivered, author has found for not
It is up to 140mAh/g using one-dimensional its specific capacity of lithium iron phosphate nano line that charcoal coats, this shows the control for LiFePO4 pattern
Making has certain active influence for the performance for promoting battery；Later, researcher has successfully synthesized LiFePO4 again and has received
Rice stick, nanometer sheet and nanometer plate etc. various nanostructures, in addition to the control to LiFePO4 pattern, researcher is to preparation
LiFePO4 be doped, to improve its physical and chemical performance, as the Changhuan Zhang et al. of Donghua University is delivered
Entitled " Effect of thermal treatment on the properties of electrospun LiFePO4-
Carbon nanofiber composite cathode materials for lithium-ion batteries " article,
In this article, author does reaction solution using the mixed solution of ferric lithium phosphate precursor and polyacrylonitrile, uses electrostatic spinning
Mode prepares nanowire, then by two sections of heatings, LiFePO4/C composite is obtained after carbonization, which has preferable
Electric property, initial discharge capacity at 0.5C is 146.3 mAh/g, and recycle after 100 circles still have it is preferable
Stability, it means that by the way that its electric property can also be promoted to LiFePO4 doping appropriate.
Although having used various means to carry out the regulation of electric property LiFePO4 at present, the prior art is come
It sees, the resistance of powder is still higher, and the electric property for being used for battery still has greatly improved space.
Summary of the invention
Inventor passes through to the field years of researches, it is proposed that a kind of height that low internal resistance is prepared by easy method
Performance LiFePO 4 powder, this method have the characteristics that simplicity, green, quickly prepare LiFePO 4 powder, and one-step method can obtain
To the LiFePO 4 powder of low internal resistance, by introducing function ingredients, the LiFePO4 composite granule prepared has preferable shape
Looks feature when being used as cell positive material, shows fabulous performance.
In order to more clearly illustrate the contents of the present invention, now technical solution of the present invention is described in detail as follows:
Firstly, the metal nanometer line of high length-diameter ratio is prepared using a kind of solvent-thermal method, the metal nanometer line that then will be prepared
It is uniformly mixed with lithium iron phosphate precursor solution, after the stirring of certain time, obtained mixed solution is transferred to microwave
It is reacted in reactor, after a few minutes, stops microwave reaction, after product cooled to room temperature, at centrifuge washing
Reason obtains the one-dimensional composite ferric lithium phosphate material original powder of LiFePO4 cladding metal nanometer line, later, by the LiFePO4 original powder
It is placed in microwave reactor and is sintered, and finally obtain product composite ferric lithium phosphate material, which has extremely low interior electricity
Resistance has preferable electric property.
Preferably, the metal nanometer line includes nanowires of gold, silver nanowires, nickel nano wire, zinc nano wire, tellurium nanometer
One or more of line and titanium nano wire.
Preferably, then the silver nanowires sufficiently divides it the preparation method comprises the following steps: firstly, weigh suitable silver nitrate
Be dispersed in ethylene glycol solvent, the backward solvent in suitable polyvinylpyrrolidone and sodium chloride is added, stirred in strength magnetic force
It mixes down, so that all dissolution completely, is eventually adding the regulation that a small amount of deionized water carries out reaction microenvironment to above-mentioned substance, it will be upper
It states mixed liquor to be placed in reaction kettle, reacted under proper temperature can be obtained the height that draw ratio is up to 800 after a certain period of time
Quality silver nanowires.
Preferably, the preparation of the lithium iron phosphate precursor solution is specifically includes the following steps: firstly, weigh suitable
Above-mentioned three is mixed in the solvent of certain volume, obtains uniform mixed solution by molysite, phosphorus source and lithium source, is added
The pH control of reaction system is arrived phosphoric acid between 8-10 by the regulation for carrying out pH after suitable ascorbic acid using ammonium hydroxide
The precursor solution of iron lithium.
Preferably, the source of iron includes frerrous chloride, ferrous sulfate, ferrous oxalate or ferrous nitrate and ferrous oxide
One or more of；The phosphorus source includes one of phosphorus pentoxide, diammonium hydrogen phosphate, ammonium dihydrogen phosphate or sodium phosphate
Or it is several；The lithium source includes one or more of lithia, lithium hydroxide, lithium carbonate or lithium acetate.
Compared with prior art, the present invention achieves following beneficial technical effect:
1), by simple microwave reaction, novel LiFePO4 cladding metal nanometer line composite material, this method have been prepared
Have the characteristics that easy to operate, environmentally protective and yield is high, at low cost；
2), this process avoids the uses of toxic reagent, and it is more energy-efficient to use microwave reaction to have compared with reactions such as hydro-thermals
Advantage；
3), coating silver nanowire composite material by LiFePO4 prepared by this method has excellent electric property, the powder
Resistivity down to 1.2 Ω/cm, according to the understanding of inventor, the production of the producers such as the current German side of the numeric ratio, state pavilion, Rett
Powder is all low, has significant progress.
Detailed description of the invention
Fig. 1 silver nanowires scanning electron micrograph prepared by the present invention；
The silver nanowires@composite ferric lithium phosphate material high power transmission electron microscope photo of Fig. 2 core-shell structure prepared by the present invention；
The silver nanowires@composite ferric lithium phosphate material low power transmission electron microscope photo of Fig. 3 core-shell structure prepared by the present invention；
High power after the silver nanowires@composite ferric lithium phosphate material microwave sintering of Fig. 4 core-shell structure prepared by the present invention transmits electricity
Mirror photo；
Low power after the silver nanowires@composite ferric lithium phosphate material microwave sintering of Fig. 5 core-shell structure prepared by the present invention transmits electricity
Mirror photo；
The charging and discharging curve of the silver nanowires@composite ferric lithium phosphate material of Fig. 6 core-shell structure prepared by the present invention.
Specific embodiment
Further description of the technical solution of the present invention below, but is not so limited, all to the technology of the present invention
Scheme is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered in the present invention
Protection scope in.
The preparation of metal nanometer line, by taking silver nanowires as an example, firstly, the silver nitrate of 1.58g is weighed, at 60 DEG C, by it
It is substantially dissolved in the ethylene glycol of 40ml, then above-mentioned solution is down to room temperature, then the polyvinylpyrrolidone of 1g is added thereto
Magnetic agitation is carried out with 0.1g sodium chloride, until all dissolution completely, obtains a kind of orange-yellow anti-after reactant is completely dissolved
Mother liquor is answered, the deionized water that 0.1ml is added in Xiang Shangshu reaction mother liquor stirs evenly, and obtained solution is transferred to reaction kettle
In, reacting 10 hours at 160 DEG C can be obtained the silver nanowires that draw ratio is up to 800.
Embodiment 1
Step 1) takes the silver nanowires prepared several, and the silver nanoparticle that concentration is 0.1mg/ml is configured to after being centrifugated
Line aqueous solution, for use；
Step 2, to weigh suitable ferrous oxide, diammonium hydrogen phosphate and lithium hydroxide by the stoichiometric ratio of LiFePO4 stand-by,
Load weighted above-mentioned substance is added separately in the deionized water of 50ml, stirring is sufficiently dissolved, homogeneous solution is obtained, then
1g ascorbic acid is added into above-mentioned solution, the pH of adjustment and control system is 8, above-mentioned solution is placed in microwave reaction instrument carry out it is micro-
Wave-hydro-thermal reaction, wherein the power of microwave reactor is 800W, reaction time 20min；After reaction by product nature
It is cooled to room temperature.
The above-mentioned product prepared is carried out centrifuge washing by step 3), can be obtained most after then carrying out microwave sintering again
Final product.
Embodiment 2
Step 1) takes the silver nanowires prepared several, and the silver nanoparticle that concentration is 0.2mg/ml is configured to after being centrifugated
Line aqueous solution, for use；
Step 2, to weigh suitable ferrous oxide, diammonium hydrogen phosphate and lithium hydroxide by the stoichiometric ratio of LiFePO4 stand-by,
Load weighted above-mentioned substance is added separately in the deionized water of 50ml, stirring is sufficiently dissolved, homogeneous solution is obtained, then
1g ascorbic acid is added into above-mentioned solution, the pH of adjustment and control system is 9, above-mentioned solution is placed in microwave reaction instrument carry out it is micro-
Wave-hydro-thermal reaction, wherein the power of microwave reactor is 800W, reaction time 20min；After reaction by product nature
It is cooled to room temperature.
The above-mentioned product prepared is carried out centrifuge washing by step 3), can be obtained most after then carrying out microwave sintering again
Final product.
Embodiment 3
Step 1) takes the silver nanowires prepared several, and the silver nanoparticle that concentration is 0.1mg/ml is configured to after being centrifugated
Line aqueous solution, for use；
Step 2, to weigh suitable ferrous oxide, diammonium hydrogen phosphate and lithium hydroxide by the stoichiometric ratio of LiFePO4 stand-by,
Load weighted above-mentioned substance is added separately in the deionized water of 50ml, stirring is sufficiently dissolved, homogeneous solution is obtained, then
1g ascorbic acid is added into above-mentioned solution, the pH of adjustment and control system is 10, and above-mentioned solution is placed in microwave reaction instrument and is carried out
Microwave-hydro-thermal reaction, wherein the power of microwave reactor is 800W, reaction time 20min；After reaction certainly by product
So it is cooled to room temperature.
The above-mentioned product prepared is carried out centrifuge washing by step 3), can be obtained most after then carrying out microwave sintering again
Final product.
Embodiment 4
Step 1) takes the silver nanowires prepared several, and the silver nanoparticle that concentration is 0.1mg/ml is configured to after being centrifugated
Line aqueous solution, for use；
Step 2, to weigh suitable ferrous oxide, diammonium hydrogen phosphate and lithium hydroxide by the stoichiometric ratio of LiFePO4 stand-by,
Load weighted above-mentioned substance is added separately in the deionized water of 50ml, stirring is sufficiently dissolved, homogeneous solution is obtained, then
1g ascorbic acid is added into above-mentioned solution, the pH of adjustment and control system is 8, above-mentioned solution is placed in microwave reaction instrument carry out it is micro-
Wave-hydro-thermal reaction, wherein the power of microwave reactor is 800W, reaction time 10min；After reaction by product nature
It is cooled to room temperature.
The above-mentioned product prepared is carried out centrifuge washing by step 3), can be obtained most after then carrying out microwave sintering again
Final product.
Embodiment 5
Step 1) takes the silver nanowires prepared several, and the silver nanoparticle that concentration is 0.05mg/ml is configured to after being centrifugated
Line aqueous solution, for use；
Step 2, to weigh suitable ferrous oxide, diammonium hydrogen phosphate and lithium hydroxide by the stoichiometric ratio of LiFePO4 stand-by,
Load weighted above-mentioned substance is added separately in the deionized water of 50ml, stirring is sufficiently dissolved, homogeneous solution is obtained, then
1g ascorbic acid is added into above-mentioned solution, the pH of adjustment and control system is 8, above-mentioned solution is placed in microwave reaction instrument carry out it is micro-
Wave-hydro-thermal reaction, wherein the power of microwave reactor is 600W, reaction time 30min；After reaction by product nature
It is cooled to room temperature.
The above-mentioned product prepared is carried out centrifuge washing by step 3), can be obtained most after then carrying out microwave sintering again
Final product.
Embodiment 6
Step 1) takes the silver nanowires prepared several, and the silver nanoparticle that concentration is 0.2mg/ml is configured to after being centrifugated
Line aqueous solution, for use；
Step 2, to weigh suitable ferrous oxide, diammonium hydrogen phosphate and lithium hydroxide by the stoichiometric ratio of LiFePO4 stand-by,
Load weighted above-mentioned substance is added separately in the deionized water of 50ml, stirring is sufficiently dissolved, homogeneous solution is obtained, then
1g ascorbic acid is added into above-mentioned solution, the pH of adjustment and control system is 8, above-mentioned solution is placed in microwave reaction instrument carry out it is micro-
Wave-hydro-thermal reaction, wherein the power of microwave reactor is 650W, reaction time 5min；It is after reaction that product is naturally cold
But to room temperature.
The above-mentioned product prepared is carried out centrifuge washing by step 3), can be obtained most after then carrying out microwave sintering again
Final product.
Comparative example 1
Silver nanowires and LiFePO 4 powder are prepared using the above method respectively, the two is then subjected to physical mixed, is obtained
The composite material of silver nanowires and LiFePO4 physical mixed, testing its resistivity is 5.8 Ω/cm, is much higher than the application center
The silver nanowires@LiFePO 4 powder of shell structure.
Claims (6)
1. a kind of preparation method of composite ferric lithium phosphate material, it is characterised in that: firstly, preparing height using a kind of solvent-thermal method
Then the metal nanometer line prepared is uniformly mixed by the metal nanometer line of draw ratio with lithium iron phosphate precursor solution, pass through
After the stirring of certain time, obtained mixed solution is transferred in microwave reactor and is reacted, after 5-30 minutes, stopped micro-
Wave reaction, after product cooled to room temperature, is handled by centrifuge washing, obtains the one of LiFePO4 cladding metal nanometer line
The LiFePO4 original powder is placed in microwave reactor and is sintered later by dimension composite ferric lithium phosphate material original powder, and final
To product composite ferric lithium phosphate material.
2. a kind of preparation method of composite ferric lithium phosphate material according to claim 1, it is characterised in that: the metal
Nano wire includes one of nanowires of gold, silver nanowires, nickel nano wire, zinc nano wire, tellurium nano-wire and titanium nano wire or several
Kind.
3. a kind of preparation method of composite ferric lithium phosphate material according to claim 2, it is characterised in that: the Yin Na
Then rice noodles are well dispersed in ethylene glycol solvent the preparation method comprises the following steps: firstly, weigh suitable silver nitrate, backward should
Suitable polyvinylpyrrolidone and sodium chloride are added in solvent, under strength magnetic agitation, so that above-mentioned substance all dissolves
Completely, it is eventually adding the regulation that a small amount of deionized water carries out reaction microenvironment, above-mentioned mixed liquor is placed in reaction kettle, Yu Shi
It is reacted at a temperature of after a certain period of time and the high-quality silver nanowires that draw ratio is up to 800 can be obtained.
4. a kind of preparation method of composite ferric lithium phosphate material according to claim 1, it is characterised in that: the phosphoric acid
The preparation of iron lithium precursor solution is specifically includes the following steps: firstly, weigh suitable molysite, phosphorus source and lithium source, by above-mentioned three
Person mixes in the solvent of certain volume, obtains uniform mixed solution, uses ammonium hydroxide after suitable ascorbic acid is added
The pH of reaction system is controlled the precursor solution that LiFePO4 is arrived between 8-10 by the regulation for carrying out pH.
5. a kind of preparation method of composite ferric lithium phosphate material according to claim 4, it is characterised in that: the source of iron
Including frerrous chloride, ferrous sulfate, ferrous oxalate or one or more of ferrous nitrate and ferrous oxide.The phosphorus source
Including one or more of phosphorus pentoxide, diammonium hydrogen phosphate, ammonium dihydrogen phosphate or sodium phosphate.The lithium source includes oxidation
One or more of lithium, lithium hydroxide, lithium carbonate or lithium acetate.
6. LiFePO4 composite wood prepared by a kind of preparation method of composite ferric lithium phosphate material according to claim 1
Material, which is characterized in that the resistivity of the composite material powder is 1.2 Ω/cm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111564616A (en) * | 2020-05-16 | 2020-08-21 | 西安建筑科技大学 | AgNWs @ Si @ GO lithium ion battery cathode material, preparation method thereof and lithium ion battery adopting same |
| CN114883557A (en) * | 2022-03-07 | 2022-08-09 | 上海交通大学 | Preparation method of lithium iron phosphate composite positive electrode material with gold nanorods as conductive additive |
-
2018
- 2018-04-11 CN CN201810319076.9A patent/CN110364694A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111564616A (en) * | 2020-05-16 | 2020-08-21 | 西安建筑科技大学 | AgNWs @ Si @ GO lithium ion battery cathode material, preparation method thereof and lithium ion battery adopting same |
| CN114883557A (en) * | 2022-03-07 | 2022-08-09 | 上海交通大学 | Preparation method of lithium iron phosphate composite positive electrode material with gold nanorods as conductive additive |
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Application publication date: 20191022 |