CN107768623A - Amorphous TiO2Thin layer cladding three-dimensional carbon network load SnO2Nano particle composite material preparation and application - Google Patents
Amorphous TiO2Thin layer cladding three-dimensional carbon network load SnO2Nano particle composite material preparation and application Download PDFInfo
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- CN107768623A CN107768623A CN201710897993.0A CN201710897993A CN107768623A CN 107768623 A CN107768623 A CN 107768623A CN 201710897993 A CN201710897993 A CN 201710897993A CN 107768623 A CN107768623 A CN 107768623A
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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
- H01M4/366—Composites as layered products
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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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- 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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
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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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
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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 present invention relates to a kind of amorphous TiO2Thin layer cladding three-dimensional carbon network load SnO2Nano particle composite material, it is characterised in that size<10nm SnO2Nano particle uniform load is on three-dimensional carbon network, the amorphous TiO with being coated on carbon-coating surface simultaneously2Layer forms sandwich structure.The preparation method of above-mentioned material is provided simultaneously.
Description
Technical field
The present invention relates to a kind of amorphous TiO2Thin layer cladding three-dimensional carbon network load SnO2The preparation of nano particle composite material
With application, belong to sodium ion secondary battery electrode material field.
Background technology
Since 21 century, the economic rapid development of countries in the world, and because today's society is to fossil energy (coal, oil, day
Right gas etc.) height rely on so that fossil energy is increasingly exhausted, and the mankind will face unprecedented energy crisis.On the other hand,
While fossil energy largely consumes, substantial amounts of carbon dioxide can be discharged and produce substantial amounts of pernicious gas and particulate pollutant,
The problems such as generation of these materials can bring serious atmosphere pollution and climate change.In face of increasingly urgent energy crisis and ring
Border problem, human society need the adjustment and transition for carrying out energy resource structure badly, are to solve using electric drive substitution fossil energy driving
A kind of effective ways of problem above.
Rechargeable battery is as a kind of efficient electrochemical energy storing device, in the great development prospect in electric drive field.Wherein,
Lithium ion battery is by its energy density is high, operating voltage is high, energy conversion rate is high, self-discharge rate is low, cost is low, cycle life
The advantages that long, communication tool used in mankind's daily life and other portable electronics markets have been captured rapidly.It is another
Aspect, with the continuous development of lithium ion battery technology and electronic equipment market, lithium resource problem increasingly highlights.Elemental lithium is on ground
Content in shell only has about 0.002%, while its distribution has serious regional differences, and these factors will cause lithium-ion electric
Pond faces serious resource and Cost Problems in the development and application in future.And it is located at the sodium element of same main group with elemental lithium
Content in the earth's crust is but up to 2.7%, while sodium element is widely distributed all over the world, and this make it that its price is much low
In the price of lithium.Have benefited from aboundresources and the low advantage of cost, sodium-ion battery be increasingly becoming the research of current secondary battery and
The new lover of exploitation.However, the radius of sodium ion is more than the radius of ion, this gives the selection band of electrode material especially negative material
Very big difficulty is carried out, the electrode material that many is applied to lithium ion battery can not be applied to sodium-ion battery.Therefore, research and development are suitable
For the electrode material of sodium-ion battery, build high performance sodium-ion battery, by be effectively reduced secondary battery system into
This, promotes extensive energy storage and the development of electric automobile industry.
Metal oxide source materials are enriched, and cost is cheap, and by polyelectron conversion storage sodium reaction theory specific capacity compared with
Height, the extensive concern of researcher is obtained.Wherein, Sn base oxides (SnO, SnO2) when for sodium-ion battery negative pole, with
The effect of storage sodium is played jointly by means of conversion reaction and alloying reaction and there is higher specific capacity.At the same time, Sn base oxides
Also there is the features such as storage sodium current potential is relatively low, nontoxic.Based on above-mentioned consideration, Sn base oxides electrochemical energy storage field by
Extensive concern and research.However, its practical application is bad by self-conductive, ion transportation is slow, stores up sodium process
The limitation for the shortcomings of middle Volume Changes are big.In order to solve above mentioned problem existing for Sn base oxides, current research persons mainly will
The research of Sn base oxides is concentrated in two kinds of approach of nanosizing and Composite.Nanosizing is intended to improve the microstructure of material,
Promote the transmission of electronics and ion in the material so as to reach, improve the purpose of material structure stability；Composite is then intended to take
It is long to mend short, the advantage of each part of bonded composite, cooperative effect is produced, reaching improves integral material practical usability
The purpose of energy.
The content of the invention
It is an object of the invention to provide a kind of amorphous TiO2Thin layer cladding three-dimensional carbon network load SnO2Nano-particles reinforcement material
Expect the preparation method of material.The preparation method process is simple, can volume production, resulting materials have good as sodium-ion battery negative pole
Charge-discharge performance, high rate performance and stability, have a extensive future.Technical scheme is as follows：
Amorphous TiO2Thin layer cladding three-dimensional carbon network load SnO2Nano particle composite material, it is characterised in that size<
10nm SnO2Nano particle uniform load is on three-dimensional carbon network, the amorphous TiO with being coated on carbon-coating surface simultaneously2Layer is formed
Sandwich structure.
The preparation method of the three-dimensional grapheme network structure load carbon covered stannum rice material of said structure includes following step
Suddenly：
(1) prepared by presoma
According to (1-1.5):(20-30):The mol ratio of (150-200), prepare Tin tetrachloride pentahydrate, citric acid and
The precursor solution of sodium chloride, and required precursor powder is made by the way of spray drying.
(2) three-dimensional carbon network load SnO2The preparation of nano particle composite material
Take precursor powder to be laid in Noah's ark, Noah's ark be steadily positioned over to high temperature process furnances flat-temperature zone, close tube furnace,
Using Ar as protective atmosphere, in-furnace temperature is risen to 600 DEG C with 10 DEG C/min programming rate, is incubated 2h to complete material
Calcining, the powder after calcining is cooled to room temperature under Ar protection afterwards, takes out sample, washing removes NaCl templates, obtained
To three-dimensional carbon network load SnO2Nano particle composite material.
(3) amorphous TiO2Thin layer cladding three-dimensional carbon network load SnO2The preparation of nano particle composite material
By three-dimensional carbon network load SnO2Nano particle composite material powder is scattered in absolute ethyl alcohol, is configured to concentration and is
0.001-0.003g/ml dispersion liquid A, then according to (100-120):(0.4-0.5):The volume ratio of (0.2-0.6) claims respectively
Dispersion liquid A, concentrated ammonia liquor (25wt%), butyl titanate are taken, first dispersion liquid A and concentrated ammonia liquor are mixed, finally instill butyl titanate, and
After carrying out high-speed stirred at 40 DEG C -60 DEG C, filter and obtain black powder, powder is placed in tube furnace, under an ar atmosphere,
300 DEG C of insulation 4h, it is amorphous TiO to obtain final product2Thin layer cladding three-dimensional carbon network load SnO2Nano-particles reinforcement material
Material.
The present invention utilizes template pyrolysismethod, prepares that lamella is very thin, and is self-assembled into the carbon network of three-dimensional structure, while
Its area load has zero dimension SnO2Nano particle, it is follow-up to combine hydrolysis control methods, in the amorphous of material surface cladding very thin thickness
TiO2Layer.This material is realized to SnO in structure2The interlayer cladding of particle, Sn base oxides are effectively prevent in storage sodium mistake
Huge Volume Changes in journey.The present invention has advantages below：The present invention prepares amorphous TiO using raw material cheap and easy to get2It is thin
Layer cladding three-dimensional carbon network load SnO2Nano particle composite material, cost is cheap, and course of reaction is simple, controllability is strong.Simultaneously
The material structure is homogeneous, and pattern is excellent, realizes the cooperative effect of multiple material, excellent performance, for sodium-ion battery negative pole
With excellent high rate performance and fabulous cycle performance, circulated 2000 times under 1000mA/g current density and remain to keep
More than 230mAh/g specific capacity, and still keep under 10A/g high current density 145mAh/g specific capacity.
Brief description of the drawings
Fig. 1 is the amorphous TiO that the embodiment of the present invention 2 obtains2Thin layer cladding three-dimensional carbon network load SnO2Nano-particles reinforcement
The SEM photograph of material.From this view it is apparent that three-dimensional carbon network morphology.
Fig. 2 is the amorphous TiO that the embodiment of the present invention 2 obtains2Thin layer cladding three-dimensional carbon network load SnO2Nano-particles reinforcement
The SEM photograph of material.From this view it is apparent that TiO2Thin layer clad structure.
Fig. 3 is the amorphous TiO that the embodiment of the present invention 2 obtains2Thin layer cladding three-dimensional carbon network load SnO2Nano-particles reinforcement
The TEM photos of material.
Fig. 4 is the amorphous TiO that the embodiment of the present invention 2 obtains2Thin layer cladding three-dimensional carbon network load SnO2Nano-particles reinforcement
The TEM photos of material.From this view it is apparent that TiO2Thin layer is made up of fine particle.
Fig. 5 is the amorphous TiO that the embodiment of the present invention 2 obtains2Thin layer cladding three-dimensional carbon network load SnO2Nano-particles reinforcement
The XRD spectrum of material.
Fig. 6 is the amorphous TiO that the embodiment of the present invention 2 obtains2Thin layer cladding three-dimensional carbon network load SnO2Nano-particles reinforcement
The Laman collection of illustrative plates of material.
Fig. 7 is the amorphous TiO obtained using the embodiment of the present invention 22Thin layer cladding three-dimensional carbon network load SnO2Nano particle
The charge-discharge performance figure of sodium-ion battery negative pole made from composite, in figure：- ■-is charging curve ,-●-be
Discharge curve.
Fig. 8 is the amorphous TiO obtained using the embodiment of the present invention 22Thin layer cladding three-dimensional carbon network load SnO2Nano particle
The charge-discharge magnification performance map of sodium-ion battery negative pole made from composite, in figure：- ■-is charging curve ,-●-be
Discharge curve.
Embodiment
The particular content of the present invention is described as follows with reference to specific embodiment：
Embodiment 1：
30g sodium chloride, 1.80g Tin tetrachloride pentahydrates and 3.60g citric acids are weighed, 200mL deionized waters is added and prepares
Mixed solution；Precursor powder is obtained using spray drying process.Take 10g precursor powders to be laid in Noah's ark, Noah's ark is put down
Surely it is positioned over high temperature process furnances flat-temperature zone.Using Ar as protective atmosphere, and with 10 DEG C/min programming rate by in-furnace temperature liter
To 600 DEG C, 2h is incubated to complete the calcining of material.Powder is taken out, NaCl templates is removed with deionized water, obtains three-dimensional carbon net
Network loads SnO2Nano particle composite material.Take 0.1g three-dimensional carbon network loads SnO2Nano particle composite material powder, is scattered in
Dispersion liquid is obtained in 100mL absolute ethyl alcohols, then to dropwise addition 0.4mL concentrated ammonia liquors in dispersion liquid, and stirs 30min.Finally take
0.2mL butyl titanates are added dropwise in dispersion liquid, and carry out high-speed stirred to mixed solution at 50 DEG C, after reacting 12h, are taken out
Filter obtains black powder.Gained powder is placed in tube furnace, under an ar atmosphere, 300 DEG C of insulation 4h, obtains final product
As amorphous TiO2Thin layer cladding three-dimensional carbon network load SnO2Nano particle composite material.
Embodiment 2：
30g sodium chloride, 1.80g Tin tetrachloride pentahydrates and 3.60g citric acids are weighed, 200mL deionized waters is added and prepares
Mixed solution；Precursor powder is obtained using spray drying process.Take 10g precursor powders to be laid in Noah's ark, Noah's ark is put down
Surely it is positioned over high temperature process furnances flat-temperature zone.Using Ar as protective atmosphere, and with 10 DEG C/min programming rate by in-furnace temperature liter
To 600 DEG C, 2h is incubated to complete the calcining of material.Powder is taken out, NaCl templates is removed with deionized water, obtains three-dimensional carbon net
Network loads SnO2Nano particle composite material.Take 0.1g three-dimensional carbon network loads SnO2Nano particle composite material powder, is scattered in
Dispersion liquid is obtained in 100mL absolute ethyl alcohols, then to dropwise addition 0.4mL concentrated ammonia liquors in dispersion liquid, and stirs 30min.Finally take
0.4mL butyl titanates are added dropwise in dispersion liquid, and carry out high-speed stirred to mixed solution at 50 DEG C, after reacting 12h, are taken out
Filter obtains black powder.Gained powder is placed in tube furnace, under an ar atmosphere, 300 DEG C of insulation 4h, obtains final product
As amorphous TiO2Thin layer cladding three-dimensional carbon network load SnO2Nano particle composite material.
With obtained material, CMC-Na, conductive carbon black mass ratio is 70:15:15 are made into slurry, are applied to copper sheet as negative
Pole, with 1mol/L NaClO4For electrolyte, using sodium piece as to electrode, half-cell is made, its electric current in 1000mA/g is close
The lower circle of circulation 2000 of degree still keeps more than 230mAh/g specific capacity, as shown in fig. 7, and having an excellent circulation
Energy, still there is 145mAh/g specific capacity under 10A/g current density, as shown in Figure 8.
Embodiment 3：
30g sodium chloride, 1.80g Tin tetrachloride pentahydrates and 3.60g citric acids are weighed, 200mL deionized waters is added and prepares
Mixed solution；Precursor powder is obtained using spray drying process.Take 10g precursor powders to be laid in Noah's ark, Noah's ark is put down
Surely it is positioned over high temperature process furnances flat-temperature zone.Using Ar as protective atmosphere, and with 10 DEG C/min programming rate by in-furnace temperature liter
To 600 DEG C, 2h is incubated to complete the calcining of material.Powder is taken out, NaCl templates is removed with deionized water, obtains three-dimensional carbon net
Network loads SnO2Nano particle composite material.Take 0.1g three-dimensional carbon network loads SnO2Nano particle composite material powder, is scattered in
Dispersion liquid is obtained in 100mL absolute ethyl alcohols, then to dropwise addition 0.4mL concentrated ammonia liquors in dispersion liquid, and stirs 30min.Finally take
0.6mL butyl titanates are added dropwise in dispersion liquid, and carry out high-speed stirred to mixed solution at 50 DEG C, after reacting 12h, are taken out
Filter obtains black powder.Gained powder is placed in tube furnace, under an ar atmosphere, 300 DEG C of insulation 4h, obtains final product
As amorphous TiO2Thin layer cladding three-dimensional carbon network load SnO2Nano particle composite material.
Claims (2)
- A kind of 1. amorphous TiO2Thin layer cladding three-dimensional carbon network load SnO2Nano particle composite material, it is characterised in that size< 10nm SnO2Nano particle uniform load is on three-dimensional carbon network, the amorphous TiO with being coated on carbon-coating surface simultaneously2Layer is formed Sandwich structure.
- 2. the preparation method of the three-dimensional grapheme network structure load carbon covered stannum rice material of structure described in claim 1, bag Include following steps：(1) prepared by presomaAccording to (1-1.5):(20-30):The mol ratio of (150-200), prepare Tin tetrachloride pentahydrate, citric acid and chlorination The precursor solution of sodium, and required precursor powder is made by the way of spray drying.(2) three-dimensional carbon network load SnO2The preparation of nano particle composite materialTake precursor powder to be laid in Noah's ark, Noah's ark is steadily positioned over to high temperature process furnances flat-temperature zone, tube furnace is closed, with Ar As protective atmosphere, in-furnace temperature is risen to 600 DEG C with 10 DEG C/min programming rate, 2h is to complete the calcining of material for insulation, The powder after calcining is cooled to room temperature under Ar protection afterwards, takes out sample, washing removes NaCl templates, obtains three-dimensional Carbon network load SnO2Nano particle composite material.(3) amorphous TiO2Thin layer cladding three-dimensional carbon network load SnO2The preparation of nano particle composite materialBy three-dimensional carbon network load SnO2Nano particle composite material powder is scattered in absolute ethyl alcohol, is configured to concentration and is 0.001-0.003g/ml dispersion liquid A, then according to (100-120):(0.4-0.5):The volume ratio of (0.2-0.6) claims respectively Dispersion liquid A, concentrated ammonia liquor (25wt%), butyl titanate are taken, first dispersion liquid A and concentrated ammonia liquor are mixed, finally instill butyl titanate, and After carrying out high-speed stirred at 40 DEG C -60 DEG C, filter and obtain black powder, powder is placed in tube furnace, under an ar atmosphere, 300 DEG C of insulation 4h, it is amorphous TiO to obtain final product2Thin layer cladding three-dimensional carbon network load SnO2Nano-particles reinforcement material Material.
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| CN110247027A (en) * | 2018-03-09 | 2019-09-17 | 广州墨羲科技有限公司 | A kind of porous three-dimensional composite material based on carbon nanosheet |
| CN112357956A (en) * | 2020-09-28 | 2021-02-12 | 浙江理工大学 | Carbon/titanium dioxide coated tin oxide nanoparticle/carbon assembled mesoporous sphere material and preparation and application thereof |
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Application publication date: 20180306 |