CN108899541A - A kind of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material and preparation method thereof - Google Patents
A kind of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material and preparation method thereof Download PDFInfo
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- CN108899541A CN108899541A CN201810779064.4A CN201810779064A CN108899541A CN 108899541 A CN108899541 A CN 108899541A CN 201810779064 A CN201810779064 A CN 201810779064A CN 108899541 A CN108899541 A CN 108899541A
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- 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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a kind of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode materials and preparation method thereof, belong to the preparation field of lithium ion battery negative material.The negative electrode material is made of lithium magnesium silicate and zinc titanate lithium, wherein lithium magnesium silicate is coated on zinc titanate lithium surface.Described method includes following steps：(1) lithium magnesium silicate is added in warm water, stirring is to forming uniform colloidal solution；(2) zinc titanate lithium powder is added in lithium magnesium silicate colloidal solution, dries product after stirring and evenly mixing；(3) product after drying in step (2) is roasted, is cooled to room temperature to get lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material.The lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material of preparation has good electronics and ionic conductivity, it is not necessary to which carrying out carbon coating can be obtained excellent high rate performance and cycle performance.
Description
Technical field
The invention belongs to the preparation field of lithium ion battery negative material more particularly to a kind of zinc titanate lithium titanate cathode materials
Method of modifying.
Background technique
The high performance advanced electrode material of lithium ion battery tight demand.Currently, commercial Li-ion battery cathode material
Material is mainly carbon material, but carbon material cryogenic property and high rate performance are poor, and cycle life is shorter (300-500 times), and is filling
Li dendrite is easily formed in discharge process, causes safety problem.Therefore, more and more researchs focus on titanium-based negative electrode material, most
Representative is lithium titanate (Li4Ti5O12, LTO), it has the characteristics such as " zero strain ", safe, environmental-friendly, still, theoretical
Specific capacity is lower (175mAh/g), cannot sufficiently be satisfied with actual needs, thus develops negative electrode material with high performance and be still
The most important thing.Recently, a kind of emerging lithium ion battery negative material, zinc titanate lithium (Li2ZnTi3O8, LZTO), receive compared with
More concerns, it has, and maturing temperature is low, calcining time is short, non-toxic and safe, advantages of environment protection, and compared with carbon material,
Due to having three-dimensional lithium ion diffusion admittance, lithium ion diffusion is accelerated, the safety of lithium ion battery is improved；With metatitanic acid
Lithium is compared, theoretical specific capacity 229mAh/g, and specific capacity improves nearly 30%, but lithium content reduces 34.5%, mentions significantly
The high cost performance of material.However, the electronic conductivity of zinc titanate lithium titanate cathode material is poor, ionic conductivity is moderate, titanium is affected
Sour zinc lithium titanate cathode material chemical property gives full play to, especially high rate capability.
It is currently used improve zinc titanate lithium electrochemical performance means include：Material with carbon-coated surface, doping foreign ion, control
System forms special appearance, surface is modified etc..Wherein surface modification is a kind of more conventional method, but common modifying agent at
Film property and caking property are poor, it is difficult to form uniform clad on zinc titanate lithium surface, final modified effect is also difficult to ensure.Cause
This, it is necessary to a kind of method of modifying of new zinc titanate lithium is studied, to further increase the chemical property of zinc titanate lithium.
Summary of the invention
For above-mentioned problems of the prior art, the present invention is intended to provide a kind of lithium magnesium silicate coating modification zinc titanate
Lithium titanate cathode material and preparation method thereof, the characteristic that there is lithium magnesium silicate stirring in water to be readily formed homogeneous colloids solution, also
It can be coated on zinc titanate lithium surface with stronger adsorptivity and caking property, when mixing with zinc titanate lithium, form uniform clad,
Surface solid electrolyte (SEI) film is served as, the consumption of lithium ion during first charge-discharge is reduced, improves coulombic efficiency for the first time；
Meanwhile lithium magnesium silicate can also function as protective layer, the side reaction between electrolyte and zinc titanate lithium titanate cathode material be hindered, thus substantially
Degree improves the chemical property of zinc titanate lithium.
An object of the present invention is to provide a kind of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material.
The second object of the present invention is to provide a kind of preparation method of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material.
The third object of the present invention is to provide lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material and preparation method thereof
Using.
For achieving the above object, specifically, the invention discloses following technical proposals：
Firstly, the invention discloses a kind of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material, the negative electrode material by
Lithium magnesium silicate and zinc titanate lithium composition, wherein lithium magnesium silicate is coated on zinc titanate lithium surface.
Preferably, the mass ratio of the lithium magnesium silicate and zinc titanate lithium is 1:(0.005-0.06).
Secondly, the invention discloses a kind of preparation methods of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material, including
Following steps：
(1) lithium magnesium silicate is added in warm water, stirring is to forming uniform colloidal solution；
(2) zinc titanate lithium powder is added in lithium magnesium silicate colloidal solution, dries product after stirring and evenly mixing；
(3) product after drying in step (2) is roasted, is cooled to room temperature to get lithium magnesium silicate coating modification titanium
Sour zinc lithium titanate cathode material.
In step (1), the temperature of the warm water is 50-70 DEG C, preferably 60 DEG C.
In step (1), the lithium magnesium silicate concentration of aqueous solution is 0.4-10g/L.
In step (2), the mass ratio of the zinc titanate lithium and lithium magnesium silicate is 1:(0.005-0.06).
In step (3), the temperature of the drying is 100-200 DEG C, and the time is 8-20 hours.
In step (3), the maturing temperature is 650-800 DEG C, time 3-10h, preferably 700-750 DEG C, 5 hours.
In step (3), cooled to room temperature after roasting.
Preferably, the zinc titanate lithium is by lithium source, zinc source and titanium dioxide by the molar ratio 2.04 of lithium, zinc, titanium:1:3 into
The baking mixed preparation of row.
Finally, the invention also discloses lithium magnesium silicate coating modification zinc titanate lithium titanate cathode materials and preparation method thereof in energy storage
Application in material.
It is characteristic of the invention that：Modifying agent lithium magnesium silicate is soluble in warm water under stiring and forms uniform colloidal solution, glues
Knot property and adsorptivity it is stronger, can uniform adhesion in zinc titanate lithium particle surface, uniform lithium magnesium silicate is formed in high-temperature roasting
Clad；Clad can both serve as surface SEI film, and the consumption of lithium ion, can also function as protective layer when reducing initial charge, hinder
Hinder the side reaction between electrolyte and zinc titanate lithium titanate cathode material；Lithium magnesium silicate has cationic exchangeability and three-dimensional ion diffusion
Channel, convenient for the insertion and abjection of lithium ion；In addition, lithium magnesium silicate is added in liquid electrolyte as additive, can be improved
The electronic conductivity of electrolyte reaches 2 × 10-4S/cm, lithium ion transference number is up to 0.98, therefore is changed by lithium magnesium silicate cladding
Property can improve the electronics and ionic conductivity of zinc titanate lithium simultaneously, improve the chemical property of lithium titanate.
Compared with prior art, the beneficial effect that the present invention obtains is：
(1) lithium magnesium silicate is mixed in water with zinc titanate lithium titanate cathode material, is roasted in air, method letter
Single, easy to operate, environmentally protective, energy consumption is less and high production efficiency.
(2) the lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material prepared has good electronics and ionic conductivity,
Need not carry out carbon coating can be obtained excellent high rate performance and cycle performance.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 is the XRD diagram of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material made from embodiment 3.
Fig. 2 is the transmission electron microscope picture of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material made from embodiment 3.
Fig. 3 is lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material made from embodiment 3 under 100mA/g current density
Cycle performance.
Fig. 4 is the high rate performance of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material made from embodiment 3.
Fig. 5 is lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material made from embodiment 3 under 500mA/g current density
Cycle performance.
Fig. 6 is that lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material made from embodiment 3 is assembled into circulating battery 100 times
Impedance diagram.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
As background technique is introduced, the currently used means for improving zinc titanate lithium electrochemical performance include：Surface
Carbon coating, doping foreign ion, control form special appearance, surface modification etc..Wherein surface modification is a kind of more conventional
Method, but common modifying agent film forming and caking property are poor, it is difficult to uniform clad is formed on zinc titanate lithium surface, finally
Modified effect be also difficult to ensure, therefore, the present invention propose a kind of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material and its
Preparation method, the present invention is described further with reference to the accompanying drawings and detailed description.
Term " drying " refers to the technical process of removal solvent reservation solid by some way.It typically refers to be passed through hot sky
The process that moisture in material is evaporated and taken away by gas.
Term " roasting " is the reaction process that solid material carries out under conditions of high temperature does not melt.
Term " grinding " is a kind of unit operation that solid matter is turned to smaller particle.
Embodiment carries out the preparation of zinc titanate lithium first in the present invention, and preparation is used uniformly lithium carbonate, zinc acetate, nano oxygen
Change titanium as lithium source, zinc source and titanium source.Weigh lithium carbonate 2.10g, zinc acetate 6.25g, nano-titanium dioxide 6.82g in the balance,
It is uniformly mixed in deionized water, is heated to 800 DEG C or so after drying in air and roasts 5 hours, cooled to room temperature obtains
To 10g white powder, as zinc titanate lithium.
Embodiment 1
A kind of preparation method of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material, includes the following steps：
(1) 0.016g lithium magnesium silicate powder is dissolved in 60 DEG C of 40mL of warm water, and stirring is to forming uniform colloidal solution；
(2) it in the lithium magnesium silicate colloidal solution for obtaining 2g zinc titanate lithium powder addition step (1), will be produced after stirring and evenly mixing
Object is dried 12 hours at 120 DEG C；
(3) product after drying in step (2) is roasted 5 hours at 750 DEG C, cooled to room temperature is to get magnesium silicate
Lithium coating modification zinc titanate lithium titanate cathode material.
Embodiment 2
A kind of preparation method of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material, includes the following steps：
(1) 0.024g lithium magnesium silicate powder is dissolved in 60 DEG C of 40mL or so of warm water, is stirred molten to uniform colloid is formed
Liquid；
(2) it in the lithium magnesium silicate colloidal solution for obtaining 2g zinc titanate lithium powder addition step (1), will be produced after stirring and evenly mixing
Object is dried 12 hours at 120 DEG C；
(3) product after drying in step (2) is roasted 5 hours at 750 DEG C, cooled to room temperature is to get magnesium silicate
Lithium coating modification zinc titanate lithium titanate cathode material.
Embodiment 3
A kind of preparation method of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material, includes the following steps：
(1) 0.030g lithium magnesium silicate powder is dissolved in 60 DEG C of 40mL or so of warm water, is stirred molten to uniform colloid is formed
Liquid；
(2) it in the lithium magnesium silicate colloidal solution for obtaining 2g zinc titanate lithium powder addition step (1), will be produced after stirring and evenly mixing
Object is dried 12 hours at 120 DEG C；
(3) product after drying in step (2) is roasted 5 hours at 750 DEG C, cooled to room temperature is to get magnesium silicate
Lithium coating modification zinc titanate lithium titanate cathode material.
Embodiment 4
A kind of preparation method of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material, includes the following steps：
(1) 0.4g lithium magnesium silicate powder is dissolved in 40mL50 DEG C or so of warm water, and stirring is to forming uniform colloidal solution；
It (2), will after stirring and evenly mixing in the lithium magnesium silicate colloidal solution for obtaining 80g zinc titanate lithium powder addition step (1)
Product is dried 20 hours at 100 DEG C；
(3) product after drying in step (2) is roasted 5 hours at 700 DEG C, cooled to room temperature is to get magnesium silicate
Lithium coating modification zinc titanate lithium titanate cathode material.
Embodiment 5
A kind of preparation method of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material, includes the following steps：
(1) 0.36g lithium magnesium silicate powder is dissolved in 70 DEG C of 40mL or so of warm water, is stirred molten to uniform colloid is formed
Liquid；
(2) it in the lithium magnesium silicate colloidal solution for obtaining 6g zinc titanate lithium powder addition step (1), will be produced after stirring and evenly mixing
Object is dried 8 hours at 200 DEG C；
(3) product after drying in step (2) is roasted 10 hours at 650 DEG C, cooled to room temperature is to get magnesium silicate
Lithium coating modification zinc titanate lithium titanate cathode material.
Embodiment 6
A kind of preparation method of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material, includes the following steps：
(1) 0.02g lithium magnesium silicate powder is dissolved in 60 DEG C of 40mL or so of warm water, is stirred molten to uniform colloid is formed
Liquid；
(2) it in the lithium magnesium silicate colloidal solution for obtaining 2g zinc titanate lithium powder addition step (1), will be produced after stirring and evenly mixing
Object is dried 10 hours at 160 DEG C；
(3) product after drying in step (2) is roasted 3 hours at 800 DEG C, cooled to room temperature is to get magnesium silicate
Lithium coating modification zinc titanate lithium titanate cathode material.
Performance test：
X-ray diffraction (XRD) is carried out to lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material made from embodiment 3 to survey
Examination, as a result as shown in Figure 1：By comparing with standard PDF card (number 86-1512), it can be confirmed that product of roasting is zinc titanate
Lithium, since lithium magnesium silicate content is lower and crystallinity is poor, it is difficult to detect the diffraction maximum of lithium magnesium silicate.
TEM test is carried out to lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material made from embodiment 3, as a result such as Fig. 2
It is shown：It can be seen that amorphous lithium magnesium silicate is fairly evenly coated on zinc titanate lithium particle surface, and zinc titanate lithium particle
Size distribution is about 50~350nm, and the thickness of lithium magnesium silicate is about 5nm.
By lithium magnesium silicate coating modification zinc titanate lithium made from embodiment 3 and conductive agent acetylene black and binder polyvinylidene fluoride
Alkene presses 8:1:1 is fabricated to electrode, and is assembled into half-cell with lithium piece, carries out electrochemical property test, as a result as shown in Figure 3：?
150 circulations are carried out under 100mA/g current density, specific capacity is up to 236.3mAh/g, and coulombic efficiency is close to 100%.
High rate performance test is carried out to lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material made from embodiment 3, as a result
As shown in Figure 4：Under 200,400,800 and 1600mA/g current density, specific capacity be respectively 217.2,200.5,183.5 and
140.4mAh/g.As it can be seen that even if lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material is at higher current densities still with excellent
Different cyclic specific capacity.
To lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material made from the present embodiment 3 under 500mA/g current density
Cyclical stability is tested, as a result as shown in Figure 5：After 400 circulations, specific capacity 189.1mAh/g, table in cyclic process
Good stability is revealed.
Electrochemical alternate impedance spectrum has been carried out to lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material made from embodiment 3
Test (IviumStat electrochemical workstation, battery recycles 100 times first under 100mA/g current density before testing), as a result such as
Shown in Fig. 6：Compared with unmodified zinc titanate lithium, the zinc titanate lithium titanate cathode material after lithium magnesium silicate cladding is at high, intermediate frequency
Reveal lesser semicircle, biggish straight slope is showed at low frequency, is illustrated after lithium magnesium silicate coats, zinc titanate lithium
Electronic conductivity and lithium ion diffusivity are all significantly improved.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for those skilled in the art
For member, various changes and changes are possible in this application.Within the spirit and principles of this application, it is made it is any modification,
Equivalent replacement, improvement etc., should be included within the scope of protection of this application.
Claims (10)
1. application of the lithium magnesium silicate in modified ion cell negative electrode material.
2. a kind of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material, it is characterised in that：The negative electrode material is by lithium magnesium silicate
It is formed with zinc titanate lithium, wherein lithium magnesium silicate is coated on zinc titanate lithium surface.
3. lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material as claimed in claim 2, it is characterised in that：The magnesium silicate
The mass ratio of lithium and zinc titanate lithium is 1:(0.005-0.06).
4. a kind of preparation method of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material, it is characterised in that：Include the following steps：
(1) lithium magnesium silicate is added in warm water, stirring is to forming uniform colloidal solution；
(2) zinc titanate lithium powder is added in lithium magnesium silicate colloidal solution, dries product after stirring and evenly mixing；
(3) product after drying in step (2) is roasted, is cooled to room temperature to get lithium magnesium silicate coating modification zinc titanate
Lithium titanate cathode material.
5. the preparation method of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material as claimed in claim 4, it is characterised in that：
In step (1), the temperature of the warm water of the warm water is 50-70 DEG C, preferably 60 DEG C；
Preferably, in step (1), the lithium magnesium silicate concentration of aqueous solution is 0.5-10g/L.
6. the preparation method of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material as claimed in claim 4, it is characterised in that：
In step (2), the mass ratio of the zinc titanate lithium and lithium magnesium silicate is 1:(0.005-0.06).
7. the preparation method of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material as claimed in claim 4, it is characterised in that：
In step (3), the temperature of the drying is 100-200 DEG C, and the time is 8-20 hours.
8. the preparation method of lithium magnesium silicate coating modification zinc titanate lithium titanate cathode material as claimed in claim 4, it is characterised in that：
In step (3), the maturing temperature is 650-800 DEG C, and the time is 3-10 hours, preferably 700-750 DEG C, 5 hours；
Or, in step (3), cooled to room temperature after roasting.
9. such as the preparation method of the described in any item lithium magnesium silicate coating modification zinc titanate lithium titanate cathode materials of claim 4-8,
It is characterized in that：The zinc titanate lithium is by lithium source, zinc source and titanium dioxide by the molar ratio 2.04 of lithium, zinc, titanium:1:3 are mixed
Roasting preparation.
10. negative electrode material as claimed in claim 2 or claim 3 and/or such as described in any item preparation methods of claim 4-9 are being stored up
Application in energy material.
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| CN114597329A (en) * | 2022-03-21 | 2022-06-07 | 西安交通大学 | Preparation method and application of zinc sheet with surface coating |
| CN114597329B (en) * | 2022-03-21 | 2023-12-26 | 西安交通大学 | Preparation method and application of zinc sheet with surface coating |
| CN114899393A (en) * | 2022-05-30 | 2022-08-12 | 西南科技大学 | Hectorite @ zinc foil negative electrode material, preparation method and water system zinc ion battery |
| CN114899393B (en) * | 2022-05-30 | 2023-05-09 | 西南科技大学 | Hectorite@zinc foil negative electrode material, preparation method and water-based zinc ion battery |
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