CN108807923A - The preparation method of sodium-ion battery modifying titanium dioxide-graphene negative material - Google Patents
The preparation method of sodium-ion battery modifying titanium dioxide-graphene negative material Download PDFInfo
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- CN108807923A CN108807923A CN201810645248.1A CN201810645248A CN108807923A CN 108807923 A CN108807923 A CN 108807923A CN 201810645248 A CN201810645248 A CN 201810645248A CN 108807923 A CN108807923 A CN 108807923A
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Abstract
A kind of preparation method of sodium-ion battery modifying titanium dioxide-graphene negative material, includes the following steps：1）Butyl titanate is added in absolute ethyl alcohol, graphene aqueous solution is then added, stirs evenly at normal temperatures；2）By uniformly mixed step 1）Solution carry out centrifugally operated, obtained precipitation is freeze-dried, and the composite nano plate of titanium dioxide/graphene is obtained after dry；3）By step 2）The composite nano plate of obtained titanium dioxide/graphene carries out high temperature phosphorization processing in phosphorous atmosphere, obtains the composite nano plate of the titanium dioxide/graphene of phosphorus doping.In the present invention, using graphene nanometer sheet as template, obtained titanium dioxide and graphene composite nano plate, the electric conductivity of the combination electrode material is improved.Phosphorus doping can improve the sodium ion transmittability of titanium dioxide surface, improve the storage sodium performance of titanium dioxide/graphene combination electrode.
Description
Technical field
The invention belongs to sodium-ion battery fields, are related to a kind of sodium-ion battery modifying titanium dioxide-graphene cathode material
The preparation method of material.
Background technology
Economic fast development keeps demand of the human society to the energy higher and higher, and energy problem, which just gradually becomes, influences me
A major challenge of state's sustainable development of socio-economy.In order to change unreasonable energy resource structure, clean regenerative resource obtains
A large amount of exploitation is to replace conventional fossil fuel, however the extensive energy storage of renewable resource and intelligent grid are built still
The problem of being urgent need to resolve.Currently, lithium ion battery obtains in a portable device since operating voltage is high and energy density is high
To being widely applied, its application in recent years also extends on electric vehicle.But the shortage of lithium resource, it has been insufficient for
Demand of the mankind to lithium ion battery rapid growth, can not meet the requirement of extensive energy storage.Therefore novel energy storage is developed
Device body is tied to form as current research emphasis and hot issue.
Sodium element is located at same main group with elemental lithium, has many physico-chemical properties similar with elemental lithium, on this basis
It has been proposed that sodium-ion battery similar with lithium ion battery working mechanism.Meanwhile sodium rich reserves on earth, it is at low cost
Honest and clean, electrolyte range of choice is wide, has better safety, has in scale energy storage and intelligent grid construction boundless
Application prospect.
However, compared to lithium ion, sodium ion has the ionic radius of bigger, this to be mostly used in lithium ion battery
Electrode material cannot be used for sodium-ion battery, therefore there is an urgent need for research and develop the electrode material suitable for sodium-ion battery.Wherein, cathode
Material is one of sodium-ion battery critical material.The anode material of lithium-ion battery being widely studied at present includes hard
Carbon, transition metal oxide/sulfide and alloy material.Wherein, hard carbon material has specific capacity high and cycle performance
Excellent feature, but embedding sodium current potential is extremely low, and there are larger safety problem, practical application is restricted；Transition metal oxide/
Although sulfide and alloy material storage sodium capacity are high, bulk effect is serious during embedding sodium, poor circulation.
Titanium dioxide（TiO2）It is of low cost with environmental-friendly, the characteristics of stable structure.It is negative as sodium-ion battery
Pole material, storage sodium current potential is high, and safety is good, and theory storage sodium capacity is up to 335mAh g-1, it is a kind of very potential sodium ion
Cell negative electrode material.However, the electronics and ionic conductivity due to titanium dioxide are poor, insertion of the sodium ion in electrode material with
Abjection is difficult, and the titanium dioxide cathode material specific capacity actually obtained is relatively low, and there is an urgent need for improve for energy-storage property.Titanium dioxide is improved at present
The method of titanium cathode storage sodium performance mainly has following three kinds of approach：（1）Synthesis has the titanium dioxide electrodes material of nanotopography,
Such as nanometer sheet, nanosphere, nanometer rods etc., although which can improve the storage sodium performance of titanium dioxide to a certain extent,
It is also easy to produce side reaction, leads to problems such as coulombic efficiency occur relatively low；（2）The titanium dioxide carbon material outstanding with electric conductivity is answered
Close, which can with the solid electrolyte interface film of three-dimensional conductive network structure and stabilization, make coulombic efficiency for the first time and
High rate performance is improved, but still needs to find the synthetic method suitable for large-scale production；（3）Dopant impurity atoms are carried out, it should
Mode can effectively improve the ion and electron conduction of electrode material, but electrode material by increasing titania structure defect
There is still a need for raisings for the coulombic efficiency for the first time of material.
Invention content
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, it is honest and clean to provide a kind of simple process and low cost,
Raw material sources are abundant, and storage sodium capacity is high, the system of sodium-ion battery modifying titanium dioxide-graphene negative material of good cycle
Preparation Method.
In order to solve the above technical problems, technical solution proposed by the present invention is：Sodium-ion battery modifying titanium dioxide-graphite
The preparation method of alkene negative material, includes the following steps：1）Butyl titanate is added in absolute ethyl alcohol, graphite is then added
Aqueous solution stirs evenly at normal temperatures；The amount of absolute ethyl alcohol is mixed for the absolute ethyl alcohol of every gram of butyl titanate and 50-5000ml
Close, the amount that graphene aqueous solution is added is that every gram of butyl titanate is added 0.5-300ml, graphene aqueous solution a concentration of 1 ~
10mg/ml；
2）By uniformly mixed step 1）Solution carry out centrifugally operated, obtained precipitation is freeze-dried, and is obtained after dry
The composite nano plate of the titanium dioxide/graphene of good dispersion；Wet feed material freezes under freezing point when freeze-drying, makes original
Moisture in material becomes solid ice, then under vacuum environment appropriate, ice is converted into steam and is removed, then use vacuum
Water vapour coagulator in system condenses water vapour, to make material obtain drying.
3）By step 2）The composite nano plate of obtained titanium dioxide/graphene carries out in phosphorous atmosphere at high temperature phosphorization
Reason, obtains the composite nano plate of the titanium dioxide/graphene of phosphorus doping.
In the present invention, the step 1）The time of middle stirring be 1 ~ for 24 hours.
In the present invention, step 2）The time of middle freeze-drying is 12 ~ 48h.In the present invention, the step 3）In phosphorous atmosphere
In phosphorus source include sodium hypophosphite, triphenyl phosphorus and ammonium dihydrogen phosphate, these three phosphide high temperature easily decompose.
In the present invention, the parkerized heating rate of step 3 high temperature is 1-5 DEG C/min, holding temperature 200-600
DEG C, soaking time 1-10h, the logical carrier gas of phosphorous atmosphere institute is inert gas, including argon gas or nitrogen.
The electrochemistry of phosphorus doping titanium dioxide/graphene cathode prepared by the present invention stores up sodium performance test：With synthesized
Phosphorus doping titanium dioxide/graphene composite nano plate is active material, is that electrode is assembled in glove box and obtained with metallic sodium
CR2032 type sodium ion button cells.
In the present invention, using template auxiliary law synthesis of titanium dioxide/graphene composite nano plate, then in phosphorous atmosphere
Phosphorating treatment is carried out, obtained phosphorus doping titanium dioxide/graphene cathode has the following advantages：
1, using graphene nanometer sheet as template, obtained titanium dioxide and graphene composite nano plate, the combination electrode material
Electric conductivity is improved.
2, phosphorus doping can improve the sodium ion transmittability of titanium dioxide surface, and it is multiple to improve titanium dioxide/graphene
The storage sodium performance of composite electrode.The coulombic efficiency for the first time of phosphorus doping titanium dioxide/graphene electrode material prepared by this method can arrive
Up to 56%, 100 circle reversible capacity of cycle can reach 340mAh g-1, show excellent cyclical stability and storage sodium specific capacity.
3, the preparation method is of low cost, raw material rich reserves, simple for process feasible, is suitable for large-scale production.
Description of the drawings
Fig. 1 is the SEM figures of the titanium dioxide/graphene composite nano plate of phosphorus doping made from example 1.
Fig. 2 is the XRD spectra of the titanium dioxide/graphene composite nano plate of phosphorus doping made from example 1.
Fig. 3 is the titanium dioxide/graphene composite nano plate of phosphorus doping made from example 1 as sodium-ion battery cathode material
Material is in current density 100mA g-15 enclose and in current density 500mA g before lower cycle-1The 6th ~ 100 circle Capacity Plan of lower cycle.
Fig. 4 is the titanium dioxide/graphene composite nano plate of phosphorus doping made from example 1 as sodium-ion battery cathode material
Expect first charge-discharge curve.
Fig. 5 be comparison example 1 titanium dioxide/graphene composite nano plate as anode material of lithium-ion battery in electric current
Density 100mA g-15 enclose and in current density 500mA g before lower cycle-1The 6th ~ 100 circle Capacity Plan of lower cycle.
Fig. 6 is that the titanium dioxide/graphene composite nano plate of comparison example 1 fills for the first time as anode material of lithium-ion battery
Discharge curve.
Specific implementation mode
To facilitate the understanding of the present invention, present invention work more comprehensively, is meticulously described below in conjunction with preferred embodiment,
But the protection scope of the present invention is not limited to the following specific embodiments.
It should be strongly noted that when to be described as " be fixed on, be fixed in, be connected to or be communicated in " another for a certain element
When on element, it can be directly fixed, affixed, connection or be connected on another element, can also be by connecting among other
Fitting is indirectly fixed, affixed, connects or is connected on another element.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection domain.
Embodiment 1
The preparation method of the sodium-ion battery modifying titanium dioxide-graphene negative material of the present embodiment includes the following steps：1）
1g butyl titanates are added in the absolute ethyl alcohol of 240ml, the graphene that a concentration of 5mg/ml of 25ml is then added is water-soluble
Liquid stirs 8h at normal temperatures.
2）After stirring, mixed solution is subjected to centrifugally operated, obtained precipitation is freeze-dried for 24 hours, after dry
Obtain the composite nano plate of titanium dioxide/graphene.
3）The composite nano plate for the titanium dioxide/graphene that above-mentioned steps are obtained carries out phosphorating treatment, phosphorus source used
For sodium hypophosphite, argon gas is passed through as protection gas, 400 DEG C, soaking time 5h are warming up to the heating rate of 2 DEG C/min,
The composite nano plate of the titanium dioxide/graphene of phosphorus doping is obtained after cooling.Fig. 1 is the dioxy of phosphorus doping made from the present embodiment
The SEM figures for changing titanium/graphene composite nano plate, come in it can be seen from the figure that, and material morphology manufactured in the present embodiment is single, disperses
Property is good.Fig. 2 be the present embodiment made from phosphorus doping titanium dioxide/graphene composite nano plate XRD spectra, composite material with
The standard JCPDS cards of anatase are consistent, without miscellaneous peak.Fig. 3 is the titanium dioxide/graphene of phosphorus doping made from the present embodiment
Composite nano plate is as anode material of lithium-ion battery in current density 100mA g-15 enclose and in current density before lower cycle
500mA g-1The 6th ~ 100 circle Capacity Plan of lower cycle, capacity maintains 340mAh g after 100 circles recycle-1More than.Fig. 4 is this implementation
The titanium dioxide/graphene composite nano plate of phosphorus doping made from example is bent as anode material of lithium-ion battery first charge-discharge
The discharge capacity for the first time of line, material is up to 452mAh g-1, the battery implemented is at 25 DEG C of constant temperature, and battery is in 0.01V-
Charge-discharge test is carried out in 3V voltage ranges.
Comparative example 1
The composite nano plate synthetic method of titanium dioxide/graphene is that the first two steps in embodiment 1 are rapid.It can from Fig. 3 and Fig. 5
Know, the composite nano plate of the titanium dioxide/graphene of phosphorus doping for the composite nano plate of titanium dioxide/graphene,
Its chemical property is more superior, it was demonstrated that phosphorus doping can be effectively improved the electrification of the composite nano plate of titanium dioxide/graphene
Learn performance.Fig. 5 is that the titanium dioxide/graphene composite nano plate of this comparative example is close in electric current as anode material of lithium-ion battery
Spend 100mA g-15 enclose and in current density 500mA g before lower cycle-1The 6th ~ 100 circle Capacity Plan of lower cycle, after 100 circles recycle
Capacity is only 218mAh g-1.Fig. 6 is the titanium dioxide/graphene composite nano plate of this comparative example as sodium-ion battery cathode
The discharge capacity for the first time of material first charge-discharge curve, material is only 248mAh g-1, the battery implemented is in 25 DEG C of constant temperature
Under, battery carries out charge-discharge test in 0.01V-3V voltage ranges.
Embodiment 2
The preparation method of the sodium-ion battery modifying titanium dioxide-graphene negative material of the present embodiment includes the following steps：
1）1g butyl titanates are added in the absolute ethyl alcohol of 240ml, the graphite of a concentration of 5mg/ml of 25ml is then added
Aqueous solution stirs 8h at normal temperatures.
2）After stirring, mixed solution is subjected to centrifugally operated, obtained precipitation is freeze-dried for 24 hours, after dry
Obtain the composite nano plate of titanium dioxide/graphene.
3）The composite nano plate for the titanium dioxide/graphene that above-mentioned steps are obtained carries out phosphorating treatment, phosphorus source used
For sodium hypophosphite, argon gas is passed through as protection gas, 500 DEG C, soaking time 5h are warming up to the heating rate of 2 DEG C/min,
The composite nano plate of the titanium dioxide/graphene of phosphorus doping is obtained after cooling.
Embodiment 3
The preparation method of the sodium-ion battery modifying titanium dioxide-graphene negative material of the present embodiment includes the following steps：
1）1g butyl titanates are added in the absolute ethyl alcohol of 240ml, the graphite of a concentration of 5mg/ml of 10ml is then added
Aqueous solution stirs 8h at normal temperatures.
2）After stirring, mixed solution is subjected to centrifugally operated, obtained precipitation is freeze-dried for 24 hours, after dry
Obtain the composite nano plate of titanium dioxide/graphene.
3）The composite nano plate for the titanium dioxide/graphene that above-mentioned steps are obtained carries out phosphorating treatment, phosphorus source used
For sodium hypophosphite, argon gas is passed through as protection gas, 350 DEG C, soaking time 5h are warming up to the heating rate of 2 DEG C/min,
The composite nano plate of the titanium dioxide/graphene of phosphorus doping is obtained after cooling.
Embodiment 4
The present embodiment includes the following steps：
1）1g butyl titanates are added in the absolute ethyl alcohol of 240ml, the graphite of a concentration of 5mg/ml of 10ml is then added
Aqueous solution stirs 6h at normal temperatures.
2）After stirring, mixed solution is subjected to centrifugally operated, obtained precipitation carries out freeze-drying 12h, after dry
Obtain the composite nano plate of titanium dioxide/graphene.
3）The composite nano plate for the titanium dioxide/graphene that above-mentioned steps are obtained carries out phosphorating treatment, phosphorus source used
For ammonium di-hydrogen phosphate, argon gas is passed through as protection gas, 400 DEG C, soaking time 5h are warming up to the heating rate of 3 DEG C/min,
The composite nano plate of the titanium dioxide/graphene of phosphorus doping is obtained after cooling.
Embodiment 5
The present embodiment includes the following steps：
1）1g butyl titanates are added in the absolute ethyl alcohol of 240ml, the graphite of a concentration of 5mg/ml of 10ml is then added
Aqueous solution stirs 6h at normal temperatures.
2）After stirring, mixed solution is subjected to centrifugally operated, obtained precipitation carries out freeze-drying 12h, after dry
Obtain the composite nano plate of titanium dioxide/graphene.
3）The composite nano plate for the titanium dioxide/graphene that above-mentioned steps are obtained carries out phosphorating treatment, phosphorus source used
For sodium hypophosphite, argon gas is passed through as protection gas, 250 DEG C, soaking time 1h are warming up to the heating rate of 2 DEG C/min,
The composite nano plate of the titanium dioxide/graphene of phosphorus doping is obtained after cooling.
Claims (5)
1. the preparation method of sodium-ion battery modifying titanium dioxide-graphene negative material, it is characterised in that：Including following step
Suddenly：1）Butyl titanate is added in absolute ethyl alcohol, graphene aqueous solution is then added, stirs evenly at normal temperatures；It is anhydrous
The amount of ethyl alcohol is that every gram of butyl titanate is mixed with the absolute ethyl alcohol of 50-5000ml, and the amount that graphene aqueous solution is added is every gram
0.5-300ml, a concentration of 1 ~ 10mg/ml of graphene aqueous solution is added in butyl titanate；
2）By uniformly mixed step 1）Solution carry out centrifugally operated, obtained precipitation is freeze-dried, and is obtained after dry
The composite nano plate of titanium dioxide/graphene；
3）By step 2）The composite nano plate of obtained titanium dioxide/graphene carries out high temperature phosphorization processing in phosphorous atmosphere,
Obtain the composite nano plate of the titanium dioxide/graphene of phosphorus doping.
2. the preparation method of sodium-ion battery modifying titanium dioxide-graphene negative material according to claim 1, special
Sign is：The step 1）The time of middle stirring be 1 ~ for 24 hours.
3. the preparation method of sodium-ion battery modifying titanium dioxide-graphene negative material according to claim 1, special
Sign is：Step 2）The time of middle freeze-drying is 12 ~ 48h.
4. the preparation method of sodium-ion battery modifying titanium dioxide-graphene negative material according to claim 1, special
Sign is：The step 3）In phosphorus source in phosphorous atmosphere include sodium hypophosphite, triphenyl phosphorus and ammonium dihydrogen phosphate.
5. the preparation method of sodium-ion battery modifying titanium dioxide-graphene negative material according to claim 1, special
Sign is：The parkerized heating rate of step 3 high temperature is 1-5 DEG C/min, and holding temperature is 200-600 DEG C, soaking time
For 1-10h, the logical carrier gas of phosphorous atmosphere institute is inert gas, including argon gas or nitrogen.
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Cited By (8)
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| CN110400702A (en) * | 2019-04-15 | 2019-11-01 | 南京工业大学 | The composite material of a kind of extra small titanium dioxide granule and carbon and its application |
| CN111211309A (en) * | 2020-01-17 | 2020-05-29 | 上海应用技术大学 | Phosphorus-doped graphene-coated iron oxide composite material and preparation method and application thereof |
| CN111244406A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院大连化学物理研究所 | Fluorinated graphene modified titanium dioxide material, and preparation and application thereof |
| CN112520722A (en) * | 2020-12-02 | 2021-03-19 | 深圳大学 | Titanium dioxide coated biomass charcoal composite anode material and preparation method and application thereof |
| CN112794365A (en) * | 2021-01-05 | 2021-05-14 | 西南大学 | Phosphorus-doped conductive carbon-coated metal oxide composite material, preparation method thereof and application thereof in sodium-ion battery cathode material |
| CN112993246A (en) * | 2021-03-16 | 2021-06-18 | 常州大学 | High-performance sodium-ion battery negative electrode material and preparation method thereof |
| CN113206247A (en) * | 2021-03-19 | 2021-08-03 | 昆山宝创新能源科技有限公司 | Core-shell structure negative electrode material, preparation method thereof and lithium ion battery |
| CN116130608A (en) * | 2023-04-04 | 2023-05-16 | 山东科技大学 | Method for preparing titanium oxide film flexible electrode by self-assembly technology |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111244406A (en) * | 2018-11-29 | 2020-06-05 | 中国科学院大连化学物理研究所 | Fluorinated graphene modified titanium dioxide material, and preparation and application thereof |
| CN110400702A (en) * | 2019-04-15 | 2019-11-01 | 南京工业大学 | The composite material of a kind of extra small titanium dioxide granule and carbon and its application |
| CN111211309A (en) * | 2020-01-17 | 2020-05-29 | 上海应用技术大学 | Phosphorus-doped graphene-coated iron oxide composite material and preparation method and application thereof |
| CN112520722A (en) * | 2020-12-02 | 2021-03-19 | 深圳大学 | Titanium dioxide coated biomass charcoal composite anode material and preparation method and application thereof |
| CN112794365A (en) * | 2021-01-05 | 2021-05-14 | 西南大学 | Phosphorus-doped conductive carbon-coated metal oxide composite material, preparation method thereof and application thereof in sodium-ion battery cathode material |
| CN112993246A (en) * | 2021-03-16 | 2021-06-18 | 常州大学 | High-performance sodium-ion battery negative electrode material and preparation method thereof |
| CN113206247A (en) * | 2021-03-19 | 2021-08-03 | 昆山宝创新能源科技有限公司 | Core-shell structure negative electrode material, preparation method thereof and lithium ion battery |
| CN116130608A (en) * | 2023-04-04 | 2023-05-16 | 山东科技大学 | Method for preparing titanium oxide film flexible electrode by self-assembly technology |
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Application publication date: 20181113 |