CN105914368B - A kind of preparation method of silicate composite positive pole - Google Patents
A kind of preparation method of silicate composite positive pole Download PDFInfo
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- CN105914368B CN105914368B CN201610303920.XA CN201610303920A CN105914368B CN 105914368 B CN105914368 B CN 105914368B CN 201610303920 A CN201610303920 A CN 201610303920A CN 105914368 B CN105914368 B CN 105914368B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
The present invention relates to a kind of preparation methods of silicate composite positive pole, and conductive agent is immersed in concentrated nitric acid first, is stirred at 80 150 DEG C, obtains processed conductive agent；Processed conductive agent is distributed in organic solvent and obtains dispersion liquid, then dispersion liquid is heated to 120 180 DEG C, then add in the aqueous solution of ferric source and is reacted, obtains presoma；Obtained presoma, lithium source and silicon source are added to the water and mixed, adds organic acid complexing agent, stirring is until form gel；By obtained gel drying, grinding, be then sintered under gas shield at 500 900 DEG C, cool down, grind after obtain silicate composite positive pole.The silicate composite positive pole of the present invention has three-dimensional porous structure and good conductive capability, has higher charge/discharge capacity and good high rate performance, is a kind of potential high performance lithium ion battery anode material.
Description
Technical field
The present invention relates to lithium ion battery material technical field more particularly to a kind of preparations of silicate composite positive pole
Method.
Background technology
With the development of society and the continuous progress of human civilization, demand sharp increase of the people to portable energy source is right
Its performance requirement is higher and higher.In addition, electric vehicle by as the replacer of 21st century potential gasoline driven automobile and
It receives much attention, and mobile power system is to restrict the key technology of electric vehicle industry development.But major part mobile power at present
Positive electrode actual specific capacity it is relatively low, the capacity for improving lithium ion cell positive be research key problem.
Since two thousand five, with ferric metasilicate lithium (Li2FeSiO4) and manganese silicate of lithium (Li2MnSiO4) be representative silicate
Anode is concerned due to its higher energy density.These silicate materials theoretically can with two lithium ions of deintercalation, than
Capacity is up to 330mAh.g-1, it is current be commercialized positive electrode 2 times.Moreover, they also have ABUNDANT NATUREAL RESOURSES, cost
It is cheap, environmental-friendly, be readily synthesized and the advantages that high security.Due to Li2MnSiO4Structure is gradually amorphous in cyclic process
Change and lose most of electrochemical characteristic, therefore, Li2FeSiO4It is the material for most having application prospect in silicate anodal.
But Li2FeSiO4Electronic conductivity it is extremely low, the solid-state diffusion of lithium ion is also very slow, therefore material charge and discharge process
In dynamic polarization it is serious, it is difficult to obtain actual high power capacity.In order to improve Li2FeSiO4The actual capacity of material, researchers
Devise a variety of modified schemes.These schemes mainly include reducing scantling, ion doping, compound etc. with carbon material.Application
Number the method for preparing nanoporous silicic acid iron lithium is disclosed for 201510061167.3 Chinese patent, nano material can shorten
Lithium ion transport distance, so as to improve electrode reaction rate；The Chinese patent of Application No. 201210207841.0 discloses vanadium
The method that doping improves ferric metasilicate lithium electronic conduction ability；The Chinese patent of Application No. 201410136971.9 discloses graphite
The method that alkene coats ferric metasilicate lithium；Guan et al. also reported that one kind passes through SiO2Middle of the road prepares Li2FeSiO4With carbon nanometer
Manage the method (J.Mater.Chem.2012,22,18797) of (CNT) composite construction.Graphene and the compound of carbon nanotubes all may be used
To be effectively improved the electronic conduction ability of material system, so as to improve Li2FeSiO4Charge/discharge capacity, but to the ion of material
The improvement of conductive capability is still limited.Therefore, developing low cost, high power capacity, environment amenable lithium ion battery becomes movement
The problem of power industry urgent need to resolve.
In view of drawbacks described above, the designer is actively subject to research and innovation, to found a kind of silicate composite positive pole
Preparation method, make it with more the utility value in industry.
The content of the invention
In order to solve the above technical problems, the object of the present invention is to provide a kind of preparation sides of silicate composite positive pole
Method, the three-dimensional porous structure of the silicate composite positive pole improve the conductive capability of material and the transmission performance of lithium ion,
So that the silicate composite positive pole has higher charge/discharge capacity and good high rate performance.
A kind of preparation method of silicate composite positive pole of the present invention, comprises the following steps：
(1) conductive agent is immersed in concentrated nitric acid, is stirred at 80-150 DEG C, obtain processed conductive agent；
(2) step (1) processed conductive agent is distributed in organic solvent and obtains dispersion liquid, then dispersion liquid is heated to
It 120-180 DEG C, then adds in the aqueous solution of ferric source and is reacted, obtain presoma；
(3) presoma, lithium source and silicon source that step (2) obtains are added to the water and mixed, then add organic acid
Complexing agent, stirring is until form gel；
(4) gel drying that obtains step (3), grinding, are then sintered under gas shield at 500-900 DEG C, cold
But silicate composite positive pole is obtained after, grinding.
Further, conductive agent is carbon nanotubes, and the mass fraction that conductive agent accounts for silicate composite positive pole is 2-
30%.
Further, in step (2), source of iron is one kind in ferric nitrate, ferrous acetate, ironic citrate and ferrous oxalate
It is or several.
Further, in step (2), organic solvent is ethylene glycol, diethylene glycol, glycerine or N, N '-dimethyl first
One kind in amide.
Further, in step (3), lithium source is one or more of lithium carbonate, lithium acetate and lithium hydroxide.
Further, in step (3), silicon source is one kind or several in silica, tetraethyl orthosilicate and lithium metasilicate
Kind.
Further, in step (3), organic acid complexing agent is ascorbic acid, acetic acid, tartaric acid, citric acid and poly- third
One or more of olefin(e) acid.
Further, in step (3), stirred at 50-80 DEG C.
Further, in step (4), gas is nitrogen and/or argon gas.
Further, the molar ratio of iron, lithium and silicon is 0.95-1.05 in silicate composite positive pole:1.9-2.2:
0.95-1.05。
According to the above aspect of the present invention, the present invention has the following advantages：The silicate composite positive pole include internal layer for CNT cores,
Outer layer is Li2FeSiO4Coaxial construction；By introducing carbon nanotubes in material structure, three-dimensional cross-linked porous structure is built,
Shorten the diffusion path of lithium ion, improve ion conduction rate；CNT coaxial constructions provide fast path for electron-transport, carry
High electron transfer rate accelerates the charge-discharge power process of material；The method of the present invention is easy to operate, and sintering time is short,
Energy loss is few, of low cost, and prepared silicate composite positive pole has higher charge/discharge capacity and good times
Rate performance, has a good application prospect.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, below with presently preferred embodiments of the present invention and coordinate attached drawing be described in detail as after.
Description of the drawings
Fig. 1 is the X-ray diffractogram of ferric metasilicate lithium composite positive pole prepared by the embodiment of the present invention 1；
Fig. 2 is the scanning electron microscope diagram of ferric metasilicate lithium composite positive pole prepared by the embodiment of the present invention 1；
Fig. 3 is the charging and discharging curve figure of ferric metasilicate lithium composite positive pole prepared by the embodiment of the present invention 1；
Fig. 4 is the charging and discharging curve figure of ferric metasilicate lithium composite positive pole prepared by the embodiment of the present invention 2.
Specific embodiment
With reference to the accompanying drawings and examples, the specific embodiment of the present invention is described in further detail.Implement below
Example is not limited to the scope of the present invention for illustrating the present invention.
Embodiment 1
2g carbon nanotubes (CNT) is taken to be immersed in concentrated nitric acid, when stirring 5 is small at 80 DEG C；0.5g concentrated nitric acids is taken to treat
Carbon nanotubes be dispersed in ethylene glycol, be warming up to 170 DEG C, add in ferrous acetate aqueous solution while stirring, and continue to stir
Mix 1 it is small when, obtain coaxial presomas of the CNT with FeOOH；Above-mentioned coaxial presoma is pressed with lithium acetate, silica
Fe:Li:The molar ratio of Si is 1:2.2:1 mixes in deionized water, then adds in tartaric acid, and the molar ratio of tartaric acid and Fe are
2:1, form colloidal sol when stirring 3 is small at 80 DEG C；Continue stirring 9 it is small when, formed gel；It by gel drying, grinds, then in argon
Under gas shielded when 650 DEG C of calcination 24 are small, ferrosilicon silicate of lithium composite positive pole is obtained after cooling, grinding.Such as Fig. 1 and Fig. 2 institutes
Show, the X-ray diffraction pattern of the material meets orthorhombic crystal phase, and pattern is three-dimensional porous structure.Charge-discharge test shows that this is compound
The discharge capacity of material reaches 221mAh.g-1, as shown in Figure 3.
Embodiment 2
2g carbon nanotubes (CNT) is taken to be dipped into concentrated nitric acid, when stirring 2 is small at 150 DEG C；0.2g concentrated nitric acids is taken to treat
CNT be dispersed in glycerine, be warming up to 130 DEG C, add in iron nitrate aqueous solution while stirring, and continue stirring 3 it is small when,
Obtain coaxial presomas of the CNT with FeOOH；Above-mentioned coaxial presoma and lithium acetate, tetraethyl orthosilicate are pressed into Fe:Li:
The molar ratio of Si is 1:2.05:1 mixes in deionized water, then adds in ascorbic acid, and ascorbic acid is 1 with Fe molar ratios:
1, form colloidal sol when stirring 3.5 is small at 70 DEG C；Continue stirring 10 it is small when, formed gel；By gel drying, grinding, Ran Hou
It under argon gas when 700 DEG C of calcination 12 are small, then cools down, grind, obtain ferrosilicon silicate of lithium composite positive pole.As shown in figure 4, the silicon
The discharge capacity of hydrochlorate composite positive pole reaches 193mAh.g-1。
Embodiment 3
2g carbon nanotubes (CNT) is taken to be dipped into concentrated nitric acid, when stirring 3 is small at 100 DEG C；0.2g concentrated nitric acids is taken to treat
CNT be dispersed in N, in N '-dimethyl formamide, be warming up to 120 DEG C, add in ironic citrate aqueous solution while stirring, and
Continue stirring 2 it is small when, obtain coaxial presomas of the CNT with FeOOH；By above-mentioned coaxial presoma and lithium hydroxide, positive silicon
Sour tetra-ethyl ester presses Fe:Li:The molar ratio of Si is 1:2.1:0.95 mixes in deionized water, then adds in citric acid, citric acid
Molar ratio with Fe is 2:1, form colloidal sol when stirring 8 is small at 50 DEG C；Continue to obtain gel when stirring 24 is small；Gel is done
Dry, grinding then under argon hydrogen mixture when 800 DEG C of calcination 3 are small, then cools down, grinds, it is compound just to obtain ferrosilicon silicate of lithium
Pole material.The discharge capacity of the silicate composite positive pole reaches 182mAh.g-1。
Embodiment 4
Take 1.5g carbon nanotubes (CNT) in concentrated nitric acid 120 DEG C stirring 4 it is small when；Take the processed CNT of 0.3g concentrated nitric acids equal
It is even to be scattered in diethylene glycol, 180 DEG C are warming up to, adds in the acidic aqueous solution of ferrous oxalate while stirring, and it is small to continue stirring 4
When, obtain coaxial presomas of the CNT with FeOOH；Above-mentioned coaxial presoma and lithium metasilicate are pressed into Fe:Li:The molar ratio of Si
For 0.95:2:1.05 mix in deionized water, then add in acetic acid, persistently stirred at 80 DEG C 24 it is small when form gel；It will
Obtained gel drying, grinding then under a nitrogen when 900 DEG C of calcination 0.5 are small, then cool down, grind, obtain ferrosilicon silicate of lithium
Composite positive pole.The discharge capacity of the silicate composite positive pole is 177mAh.g-1。
Embodiment 5
When by 1.5gCNT, stirring 5 is small at 120 DEG C in concentrated nitric acid；The processed CNT of 0.3g concentrated nitric acids is taken to be dispersed in
In ethylene glycol, be warming up to 160 DEG C, while stirring add in ferrous acetate aqueous solution, and continue stirring 5 it is small when, obtain CNT and hydroxyl
The coaxial presoma of base iron oxide；Above-mentioned coaxial presoma and lithium acetate, silica are pressed into Fe:Li:The molar ratio of Si is
1.05:2:1.05 ratio mixes in deionized water, then adds in ascorbic acid, is formed when stirring 10 is small at 60 DEG C molten
Glue, continue stirring 10 it is small when, formed gel；By gel drying, grind, then under argon gas when 750 DEG C of calcination 6 are small, then it is cold
But, grind, obtain ferrosilicon silicate of lithium composite positive pole.The discharge capacity of the silicate composite positive pole reaches
202mAh.g-1。
The silicate composite positive pole includes ferric metasilicate lithium active material and carbon nanotube conducting agent, wherein ferric metasilicate lithium
The surface for being equably wrapped in carbon nanotubes forms coaxial material, and is further formed porous three-dimensional netted cross-linked structure；By
In with three-dimensional porous structure and good conductive capability, the silicate anode composite is with higher charge/discharge capacity and well
High rate performance, ferric metasilicate lithium composite positive pole prepared by method using the present invention has up to 221mAh.g-1Electric discharge
Capacity.
The above is only the preferred embodiment of the present invention, is not intended to limit the invention, it is noted that for this skill
For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is several improvement and
Modification, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of silicate composite positive pole, which is characterized in that comprise the following steps：
(1) conductive agent is immersed in concentrated nitric acid, is stirred at 80-150 DEG C, obtain processed conductive agent；
(2) step (1) processed conductive agent is distributed in organic solvent and obtains dispersion liquid, then the dispersion liquid is heated to
It 120-180 DEG C, then adds in the aqueous solution of ferric source and is reacted, obtain presoma；
(3) presoma, lithium source and silicon source that step (2) obtains are added to the water and mixed, then add organic acid complexing
Agent, stirring is until form gel；
(4) gel drying that obtains step (3), grinding, are then sintered at 500-900 DEG C under gas shield, cool down, grind
The silicate composite positive pole is obtained after mill.
2. the preparation method of silicate composite positive pole according to claim 1, it is characterised in that：The conductive agent is
Carbon nanotubes, the mass fraction of conductive agent described in the silicate composite positive pole are 2-30%.
3. the preparation method of silicate composite positive pole according to claim 1, it is characterised in that：In step (2),
The source of iron is one or more of ferric nitrate, ferrous acetate, ironic citrate and ferrous oxalate.
4. the preparation method of silicate composite positive pole according to claim 1, it is characterised in that：In step (2),
The organic solvent is ethylene glycol, one or more of diethylene glycol, glycerine and N, N '-dimethyl formamide.
5. the preparation method of silicate composite positive pole according to claim 1, it is characterised in that：In step (3),
The lithium source is one or more of lithium carbonate, lithium acetate and lithium hydroxide.
6. the preparation method of silicate composite positive pole according to claim 1, it is characterised in that：In step (3),
The silicon source is one or more of silica, tetraethyl orthosilicate and lithium metasilicate.
7. the preparation method of silicate composite positive pole according to claim 1, it is characterised in that：In step (3),
The organic acid complexing agent is one or more of ascorbic acid, acetic acid, tartaric acid, citric acid and polyacrylic acid.
8. the preparation method of silicate composite positive pole according to claim 1, it is characterised in that：In step (3),
It is stirred at 50-80 DEG C.
9. the preparation method of silicate composite positive pole according to claim 1, it is characterised in that：In step (4),
The gas is nitrogen and/or argon gas.
10. the preparation method of silicate composite positive pole according to claim 1, it is characterised in that：The silicate
The molar ratio of iron, lithium and silicon is 0.95-1.05 in composite positive pole:1.9-2.2:0.95-1.05.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101546828A (en) * | 2008-12-27 | 2009-09-30 | 深圳市德方纳米科技有限公司 | Nanometer ferrous silicate lithium material and preparation method thereof |
| CN103746116A (en) * | 2014-01-10 | 2014-04-23 | 国家纳米科学中心 | Carbon-coated ferrous lithium silicate anode material, as well as preparation method and application thereof |
| CN103985867A (en) * | 2014-05-19 | 2014-08-13 | 电子科技大学 | Method for preparing carbon-coated lithium iron silicate composite material |
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| JP5950389B2 (en) * | 2012-02-28 | 2016-07-13 | 株式会社豊田自動織機 | Lithium silicate compound, positive electrode active material, method for producing positive electrode active material, non-aqueous electrolyte secondary battery and vehicle equipped with the same |
| JP5901019B2 (en) * | 2012-12-18 | 2016-04-06 | 太平洋セメント株式会社 | Method for producing positive electrode active material for lithium ion battery |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101546828A (en) * | 2008-12-27 | 2009-09-30 | 深圳市德方纳米科技有限公司 | Nanometer ferrous silicate lithium material and preparation method thereof |
| CN103746116A (en) * | 2014-01-10 | 2014-04-23 | 国家纳米科学中心 | Carbon-coated ferrous lithium silicate anode material, as well as preparation method and application thereof |
| CN103985867A (en) * | 2014-05-19 | 2014-08-13 | 电子科技大学 | Method for preparing carbon-coated lithium iron silicate composite material |
Non-Patent Citations (1)
| Title |
|---|
| Qingtang Zhang et al..Nano/micro lithium transitionmetal (Fe,Mn,Co and Ni) silicate cathode materials for lithium ion batteries.《Nanotechnology》.2011,第5卷全文. * |
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