CN109659512A - A kind of flower ball-shaped TiO2/ MoO2 composite nano materials, preparation method and application - Google Patents
A kind of flower ball-shaped TiO2/ MoO2 composite nano materials, preparation method and application Download PDFInfo
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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
- H01M4/362—Composites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 invention discloses a kind of flower ball-shaped TiO2/MoO2Composite nano materials, preparation method and application.The TiO2/MoO2Composite material is by MoO2Nano particle is evenly coated at TiO2The surface of nano-cluster forms nanostructure, and the flower ball-shaped nano material that high-temperature calcination obtains further is carried out to it.When preparing the material, hydro-thermal method is used first and synthesizes sodium titanate (NaTi3O7), it then exchanges to obtain TiO by hydrogen ion2Nano-cluster precursor recycles ammonium molybdate hydrolysis to generate MoO2Nano particle is evenly coated at TiO2The surface of nano-cluster obtains flower ball-shaped nanostructure, which can be substantially reduced ion diffusion length, and can effectively adapt to volume expansion;MoO simultaneously2Superfine nano particle also contributes to reducing ion diffusion length, promotes Ion transfer, to improve the chemical property of lithium ion battery negative material.
Description
Technical field
Composite nano materials field of the present invention, in particular to a kind of flower ball-shaped TiO2/MoO2Composite nano materials, preparation side
Method and application.
Background technique
With the exhausted of three macrofossil fuel and increasingly bad problem of environmental pollution, renewable energy and clean energy resource
Exploitation it is extremely urgent.The energy increasingly becomes hot topic concerned by people, with daily life mode and pursue
Higher quality of the life is closely bound up.Therefore realize renewable energy reasonable disposition and environmentally friendly battery, be generation from now on
Particularly important one of technical field in boundary's economy.At us in sustainable renewable sources of energy development process, these energy due to
There is being difficult to the disadvantages of storing, is discontinuous and uncertain, thus to utilize on a large scale these cleanings it is friendly it is big from
Our energy is so given, then needs to design and manufacture corresponding reservoir and energy transfer machine.Therefore, lithium ion battery
It (LIB) is secondary high-efficiency battery most with prospects at present, and it is currently chemical energy storage electricity with fastest developing speed on the market
Source.Compared with traditional secondary cell, lithium ion battery has high-energy density, specific capacity height, operating voltage height, high rate performance
It gets well, good cycle, low self-discharge rate, memory-less effect, can be quickly charged and discharged, that environmentally protective and charge discharge life is long etc. is excellent
Point, it is believed that it can be used as a kind of energy storage device realizing chemical energy and electric energy and mutually converting, and is widely studied and opens in recent years
Hair, oneself is widely used in household electrical appliance, portable electronic device, power vehicle etc. at present, and is gradually related to electric car
Dynamic field.In face of increasingly serious energy environment issues, lithium ion battery applications in various fields is increasing, therefore develops
Capacity height, high power density, the new type lithium ion battery of the excellent high security of high rate performance are imperative.
Titanium dioxide (TiO2) there is chemical structure property to stablize, cheap, stable circulation performance is superior, discharge voltage
The features such as platform is high, and lithium ion intercalation/deintercalation depth is small, stroke is short, nontoxic, environmental-friendly, highly-safe, is lithium ion battery
The research hotspot of metal oxide negative electrode material.But itself be semiconductor material, electronic conductivity is low cause specific capacity it is low, times
Rate performance is poor, and lithium ion migrates wherein to be limited, and diffusion coefficient is small, if these problems cannot be resolved the lithium that will be reduced
The reality of ion battery uses.
Molybdenum dioxide (Mo02) it is a kind of cheap, environmentally friendly material, belong to monoclinic system, P21/c groups, has
There is the rutile crystalline structure of distortion, this special structure makes Mo02Conductivity with higher and fusing point, and chemistry is steady
Qualitative good, oneself attracts extensive attention in fields such as clang ion battery, supercapacitor, sensor, catalyst at present, is that one kind is answered
With a wide range of transition metal oxide material of prospect.
Lead that lithium ability is poor due to TiO2 itself, so that diffusion of the lithium ion in electrode material is restricted, because
This, the diffusion path of lithium ion can effectively be shortened by preparing the special material of pattern, increase connecing for electrode material and electrolyte
Contacting surface product, to improve the specific capacity and high rate performance of electrode material.
During insertion of the lithium ion in material is deviate from, the particle of partial size fine uniform can shorten lithium ion in solid phase
The distance of middle migration makes full use of the active material near granular center, and then improves the chemical property of material;Meanwhile material
Expect that particle is tiny, pattern is uniform but also specific surface area increases, electrolyte can more fully contact active matter when electrode reaction
Matter.Therefore, preparation method is improved, synthesis partial size is tiny, be evenly distributed is the important channel for improving its chemical property.
Summary of the invention
The purpose of the present invention is to provide a kind of flower ball-shaped TiO2/MoO2Combination electrode material and preparation method thereof.This is compound
Electrode material is by by MoO2Nano particle is evenly coated at TiO2The surface of nano-cluster obtains flower ball-shaped nanostructure, the nanometer
Structure can be substantially reduced ion diffusion length, and can effectively adapt to volume expansion;MoO simultaneously2Superfine nano particle
It also contributes to reducing ion diffusion length, promotes Ion transfer, to improve the electrochemistry of lithium ion battery negative material
Performance.
TiO provided by the invention2/MoO2Composite nano materials, by MoO2Coat TiO2It forms, is one kind in TiO2Nano-cluster
The MoO that ammonium molybdate hydrolysis generates is coated on presoma2The flower ball-shaped TiO that nano particle is formed2/MoO2Combination electrode material.
Its it is specific the preparation method is as follows:
(1) titanium dioxide P25 is dissolved in sodium hydroxide solution, with the dissolution of suitable revolving speed magnetic agitation, then will
It is transferred in polytetrafluoroethyllining lining kettle, and 130 DEG C of reactions are for 24 hours.It is cooled to room temperature to product, spends ion-cleaning for several times.Most
Afterwards, by obtained sample in diluted HNO3Stirring carries out hydrogen ion exchange in solution, is then centrifuged for washing for several times, and in vacuum
It is further dried to obtain TiO in baking oven2Nano-cluster precursor.
(2) TiO that will be obtained2Nano-cluster precursor disperses in deionized water, to be ultrasonically treated 15 minutes, with suitable rotational speed
Magnetic agitation 20 minutes, ammonium molybdate and dopamine are then being added into suspension, and is continuing stirring and makes it completely dissolved, so
After ethyl alcohol is added, quickly stirring 5 minutes.Later, ammonia solution (28%-30%) is added, and the solution is continuously stirred at room temperature
It mixes 1.5 hours.Precursor is obtained by being dried in vacuo 10h twice and at 50 DEG C with ethyl alcohol centrifugation.Finally, passing through the Ar in flowing
Calcining is in atmosphere to prepare TiO2/MoO2Combination electrode material.
(3) by the flower ball-shaped TiO of synthesis2/MoO2The method that combination electrode material is prepared into serondary lithium battery is as follows: will be upper
The flower ball-shaped TiO stated2/MoO2Electrode material, acetylene black, PVDF are dissolved in NMP adhesive according to the mass ratio of 80:10:10,
Stirring forms uniform sizing material;Slurry is uniformly coated on clean copper foil paper with wet film maker, electrode slice is made, and 110
DEG C baking oven in dry;The electrode slice of drying and lithium piece are packaged into lithium battery in the glove box of argon atmosphere.
Above-mentioned TiO2Nano-cluster can also be prepared by electrospinning process.
The first step synthesizes TiO2The pH value of supernatant is washed till about 9 when washing for the first time by nano-cluster precursor,
After hydrogen ion exchange, supernatant is washed till neutrality.
The first step synthesizes TiO2Nano-cluster precursor, the dosage of the sodium hydroxide solution are 10M;HNO3 solution
Dosage be 0.1M.
The high temperature sintering sets heating rate as 5 DEG C/min, and temperature is 750 DEG C, soaking time 180min.
The first step synthesizes TiO2Nano-cluster precursor, titanium dioxide P25 dosage are 0.4g;Deionized water dosage is
60mL;The second step TiO2/MoO2Combination electrode material, TiO2Nano-cluster precursor dosage 100mg;Deionized water dosage is
80mL;Ammonium molybdate and dopamine mass ratio are 4:1, and ammonium molybdate dosage is 0.8g;Dopamine dosage is 0.2g;Ammonia solution dosage is
1.2mL。
Compared with prior art, the invention has the following beneficial effects: when preparing the material, simplicity is used first
Hydro-thermal method synthesizes sodium titanate (NaTi3O7), it then exchanges to obtain TiO by hydrogen ion2Nano-cluster precursor.Utilize ammonium molybdate water
Solution generates MoO2Nano particle is evenly coated at TiO2The surface of nano-cluster forms unique flower-like nanostructure, which can
To be substantially reduced ion diffusion length, MoO2Superfine nano particle helps to reduce ion diffusion length, promotes Ion transfer;And
And volume expansion can be effectively adapted to, to improve the cyclical stability and high rate performance of negative electrode material.This programme
Heterosis exists: cost of material is low, simple and easy to understand, it is easy to accomplish, obtained flower ball-shaped TiO2/MoO2Combination electrode material
Epigranular, chemical property are good.
Detailed description of the invention
Fig. 1 is the flower ball-shaped TiO that embodiment 2 obtains2/MoO2The SEM of combination electrode material schemes, (a) in figure, (b), (c) and
(d) amplification factor is sequentially increased.
Fig. 2 (a) is TiO2/MoO2The XRD diagram of electrode material (b) is that flower ball-shaped TiO is applied in embodiment 12/MoO2It is multiple
First charge-discharge curve (c) and (d) of the lithium battery of composite electrode material preparation under 0.1C multiplying power are bouquet prepared by embodiment 1
Shape TiO2/MoO2Circulation figure of the combination electrode material under 0.5C multiplying power.
Fig. 3 (a) and (b) are respectively in embodiment 1 using flower ball-shaped TiO2/MoO2The secondary lithium of combination electrode material preparation
Charge/discharge capacity and charging and discharging curve of the battery under 0.1,0.2,0.5,1,2,5,10,20C multiplying power.
Specific embodiment
With reference to the accompanying drawing, specific embodiments of the present invention will be described in detail, it is to be understood that guarantor of the invention
Shield range is not limited by the specific implementation.
1 TiO of embodiment2Nano-cluster presoma
0.4gP25 is dissolved in 60mL10molL-1Sodium hydroxide solution in, with the revolving speed magnetic agitation of 400r/min
1.5h dissolution, transfers it in polytetrafluoroethyllining lining kettle, and 130 DEG C of reactions are for 24 hours.It is cooled to room temperature to product, is spent
Ion-cleaning to pH be 9.Finally, by obtained sample in diluted HNO3Solution (concentration 0.1molL-1, 80mL) in stirring
Hydrogen ion exchange is carried out, being then centrifuged for washing to pH is 7, and is further dried to obtain TiO in vacuum drying oven2Nano-cluster forerunner
Body.
2 flower ball-shaped TiO of embodiment2/MoO2The preparation of combination electrode material
The 100mgTiO that embodiment 1 is obtained2Nano-cluster presoma is dispersed in 80mL deionized water, is ultrasonically treated 15 points
Then clock 0.8g ammonium molybdate and 0.2g dopamine had been added into suspension with 400r/min revolving speed magnetic agitation 20 minutes, and
And continue stirring and make it completely dissolved, 160mL ethyl alcohol is then added, quickly stirring 5 minutes.Later, 1.2mL mass concentration is added
For 15.8molL-1, ammonia solution (28%-30%), and the solution is continuously stirred 1.5 hours at room temperature.By with ethyl alcohol
Centrifugation is dried in vacuo 10h twice and at 50 DEG C and obtains precursor.Finally, being made by calcining 750 DEG C in the Ar atmosphere of flowing
Standby TiO2/MoO2Combination electrode material.
The assembling of 3 button cell of embodiment
The flower ball-shaped TiO that embodiment 2 is synthesized2/MoO2Electrode material, acetylene black, PVDF according to 80:10:10 mass ratio
It is dissolved in NMP adhesive, stirring forms uniform sizing material;Slurry is uniformly coated on clean copper foil paper with wet film maker
Electrode slice is made, and is dried in 110 DEG C of baking oven, the electrode slice of drying is carved into the disk of 12mm simultaneously and lithium piece is in argon atmospher
Half-cell is packaged into the glove box enclosed.
Fig. 1 (a), (b), (c) and (d) TiO2/MoO2The low range and high magnification SEM image of material.It can be seen in SEM
The TiO prepared out2/MoO2Material is rendered as flower-like structure, and size is uniform.This kind of flower-like structure is conducive to increase ratio
Surface area and the more active sites of exposure, reduce the loss of ion and charge, to improve the performance of material.
Fig. 2 (a) is TiO2/MoO2The XRD diagram of electrode material, (b) the flower ball-shaped TiO to be prepared in embodiment 12/MoO2
First charge-discharge curve (c) of the combination electrode material under 0.1C multiplying power and (d) are flower ball-shaped TiO prepared by embodiment 12/MoO2
Circulation figure of the combination electrode material under 0.5C multiplying power.Successful synthesis can be clearly found out by XRD diagram diffraction maximum
TiO2/MoO2Combination electrode material.TiO2/MoO2The discharge capacity for the first time of negative electrode material reaches 1102.4mAh/g, this is because
In discharge process for the first time electrode material and electrolyte have occurred it is irreversible react, consume more electrolyte, and for the first time
Coulombic efficiency it is lower, only 56.7%.Second of discharge capacity is 556.5mAh/g, and coulombic efficiency maintains 91% left side
The right side shows the preferable invertibity of material.It can be seen that material under 0.5C multiplying power by the circulation figure of electrode material to recycle
Capacity is 451.7mAh/g after 100 times, and capacity retention ratio is 98.5% or so, it was demonstrated that flower ball-shaped TiO2/MoO2Combination electrode material
Material has preferable stable circulation performance.
Fig. 3 (a) and (b) are flower ball-shaped TiO prepared by embodiment 12/MoO2Combination electrode material 0.1,0.2,0.5,1,
2,5, the 10, charging and discharging curve under 20C multiplying power.TiO2/MoO2Electrode material is corresponding when current density is 0.1C to 20C
TiO2/MoO2The discharge capacity of electrode material be respectively 182,169mAh/g, 151mAh/g, 137mAh/g, 112mAh/g,
94mAh/g, 63mAh/g show preferable high rate performance.
Above-mentioned assembling is button cell, it is only for the secondary cell flower testing the performance of the material, however preparing
Spherical TiO2/MoO2Combination electrode material can be applied in all kinds of lithium batteries such as rectangular, button, flexible package, cylindrical battery.
Disclosed above is only specific embodiments of the present invention, and still, the present invention is not limited to this, any this field
What technical staff can think variation should all fall into protection scope of the present invention.
Claims (10)
1. a kind of flower ball-shaped TiO2/MoO2Combination electrode material, which is characterized in that the TiO2/MoO2Nano material is that one kind exists
TiO2The MoO that ammonium molybdate hydrolysis generates is coated on nano-cluster presoma2The flower ball-shaped TiO that nano particle is formed2/MoO2Compound electric
Pole material.
2. flower ball-shaped TiO according to claim 12/MoO2Combination electrode material, which is characterized in that the TiO2Nanometer
Cluster presoma is prepared by hydro-thermal method or electrospinning process.
3. flower ball-shaped TiO according to claim 22/MoO2Combination electrode material, which is characterized in that the hydro-thermal method
Specific step is as follows:
Titanium dioxide P25 is dissolved in sodium hydroxide solution, stirring and dissolving, transfers it to polytetrafluoroethyllining lining kettle
Middle carry out hydro-thermal reaction, is cooled to room temperature to product, is washed with deionized, then, by obtained sample in diluted HNO3
Stirring carries out hydrogen ion exchange in solution, finally uses deionized water centrifuge washing, and be further dried to obtain in vacuum drying oven
TiO2Nano-cluster presoma.
4. flower ball-shaped TiO according to claim 32/MoO2Combination electrode material, which is characterized in that the hydro-thermal reaction
Temperature is 130 DEG C, and the reaction time is 24 hours.
5. flower ball-shaped TiO according to claim 32/MoO2Combination electrode material, which is characterized in that the deionized water
Washing to pH value is 9, and after hydrogen ion exchange, centrifuge washing to supernatant pH is 7.
6. flower ball-shaped TiO according to claim 32/MoO2Combination electrode material, which is characterized in that the sodium hydroxide
Solution concentration is 10molL-1, when titanium dioxide p25 is added, the mass volume ratio with sodium hydroxide is 1:60;HNO3 solution is dense
Degree is 0.1molL-1。
7. a kind of flower ball-shaped TiO described in claim 12/MoO2The preparation method of combination electrode material, which is characterized in that including
Following steps:
(1) titanium dioxide P25 is dissolved in sodium hydroxide solution, stirring and dissolving transfers it in polytetrafluoroethylene (PTFE)
Hydro-thermal reaction is carried out in lining kettle, room temperature is cooled to product, is washed with deionized, then, by obtained sample diluted
HNO3Stirring carries out hydrogen ion exchange in solution, finally uses deionized water centrifuge washing, and be further dried in vacuum drying oven
Obtain TiO2Nano-cluster presoma;
(2) TiO for obtaining step (1)2Nano-cluster presoma disperses in deionized water, and sonicated, magnetic agitation obtains
TiO2Then ammonium molybdate and dopamine is added in nano-cluster presoma suspension into the suspension, and continuing stirring keeps its complete
Fully dissolved adds ethyl alcohol, and material is made to be easily dispersed, homogenize, and later, ammonia solution is added, and the solution is connected at room temperature
Continuous stirring 1.5 hours is then dried in vacuo acquisition precursor with ethyl alcohol centrifugation, finally, in Ar protective atmosphere twice and at 50 DEG C
Calcining is to prepare TiO2/MoO2Combination electrode material.
8. flower ball-shaped TiO according to claim 72/MoO2The preparation method of combination electrode material, which is characterized in that step
(2) ammonia solution concentration is 28%-30% in, and dosage 1.2mL, ammonium molybdate and dopamine mass ratio are 4:1.
9. flower ball-shaped TiO according to claim 72/MoO2The preparation method of combination electrode material, which is characterized in that step
(2) TiO for obtaining step (1) in2Sonication treatment time is 15 minutes after nano-cluster presoma is dispersed in deionized water, then
TiO was obtained with revolving speed magnetic agitation 20 minutes of 400r/min2Nano-cluster presoma suspension, calcination temperature are 750 DEG C, heating
Speed is 5 DEG C of min-1, calcination time 180min.
10. applying flower ball-shaped TiO described in claim 12/MoO2Combination electrode material prepares serondary lithium battery application.
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Cited By (3)
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Application publication date: 20190419 |