CN105789586A - SnO2/CNTs (stannic oxide/ carbon nanotubes) composite electrode material for positive electrode of sodium ion battery - Google Patents
SnO2/CNTs (stannic oxide/ carbon nanotubes) composite electrode material for positive electrode of sodium ion battery Download PDFInfo
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- CN105789586A CN105789586A CN201610187643.0A CN201610187643A CN105789586A CN 105789586 A CN105789586 A CN 105789586A CN 201610187643 A CN201610187643 A CN 201610187643A CN 105789586 A CN105789586 A CN 105789586A
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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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- 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
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method of a SnO2/CNTs (stannic oxide/ carbon nanotubes) composite electrode material for a positive electrode of a sodium ion battery. The preparation method is characterized in that water is used as a solvent; SnCl2 2H2O is used as a raw material; carboxylation CNTs are used as a carbon source; the SnO2/CNTs composite material is prepared by a hydrothermal method, the particle size of SnO2 is 5nm, and SnO2 grows at the surfaces of the CNTs. The preparation method has the advantages that the technology is simple, the preparation cycle is short, the repeatability is high, the reaction temperature is low, the production cost is reduced, and the preparation method is suitable for large-batch production and preparation.
Description
Technical field
The present invention relates to a kind of sodium-ion battery negative pole SnO2The preparation of composite, is specifically related to a kind of sodium-ion battery negative pole SnO2The preparation method of/CNTs combination electrode material.
Background technology
At present, sodium-ion battery becomes the most possible secondary cell substituting lithium ion battery due to reasons such as the low cost in its sodium source, environmental friendliness, safeties.Anode material of lithium-ion battery mainly includes carbon based negative electrodes material and titanio negative material, and they are respectively provided with good cyclical stability, but reversible capacity only has 200～300mAhg-1.And due to its limited avtive spot, capacity is difficult to improve a lot.Therefore, the negative material with high power capacity of development of new is highly significant.In the research of anticathode material, SnO2Due to high storage sodium capacity (1367mAhg-1), cause the extensive concern of battery material circle.
But, SnO2As anode material of lithium-ion battery, there is very big bulk effect, cause the powder of detached of material in charge and discharge process, reduce battery high rate performance and cyclical stability, greatly have impact on the application in practice of this kind of material.Current and carbon compound is modal a kind of raising SnO2The method of cyclical stability.Common material with carbon element has multi-walled carbon nano-tubes, Graphene etc..Multi-walled carbon nano-tubes becomes and SnO due to advantages such as its one-dimensional tubular structure, high conductivity, high-ratio surfaces2The desirable carbon source of compound.YingWang etc. adopt solvent-thermal method by SnO2The SnO prepared with multi-walled carbon nano-tubes compound2MWCNT negative material, at 50mAg-1Electric current density under, 50 times circulation after capacity may remain in 400mAhg-1(SnO2MWCNTnanocompositeasahighcapacityanodematerialforsodium-ionbatteries.ElectrochemistryCommunications.2013；29:8-11).HilalKose etc. adopt sol-gal process to be prepared for SnO2/ MWCNT composite is as lithium ion battery negative, and after 100 circulations, capacity may remain in 310mAhg-1(Sol-gelpreparationandelectrochemical characterizationofSnO2/MWCNTsanodematerialsforLi-ionbatteries.AppliedSurfaceScience.2013；275:160-167).
As can be seen here, by can be greatly enhanced the cyclical stability of electrode material with the compound of CNT, but the method that report adopts at present on the other hand is more complicated, generally require and one favourable environment of dispersed offer that some organic solvents are CNT is provided, this greatly limits it to produce in enormous quantities, and SnO in the composite of preparation2The surface of CNT can not be grown in well.Therefore a kind of preparation process of exploitation is simple, and can Effective Regulation SnO2The method of/CNTs structure has great importance.
Summary of the invention
It is an object of the invention to provide a kind of sodium-ion battery negative pole SnO2The preparation method of/CNTs combination electrode material, prepared SnO2/ CNTs combination electrode material, its SnO2Nano-particle is grown in the surface of CNTs uniformly.
For reaching above-mentioned purpose, present invention employs techniques below scheme:
1) adding in 10～80mL deionized water by 30～90mgCNTs (CNTs and CNT), after stirring, supersound process 10～120min obtains mixed liquor A；Then in described mixed liquor A, add 0.1～2.706gSnCl again2·2H2O, after stirring, supersound process 10～120min obtains mixed liquid B；
2) described mixed liquid B is transferred in politef water heating kettle, then politef water heating kettle it is placed in homogeneous reactor and at 120～230 DEG C, reacts 2～50h, reaction is cooled to room temperature after terminating, then pass through the centrifugal powder body that will be obtained by reacting separation, the powder freezing that separation obtains is dried and obtains SnO2/ CNTs combination electrode material.
Described step 1) in, SnCl2·2H2The mass ratio of O and CNTs is 4.3～90.2:1.
In described mixed liquor A, the concentration of CNTs is 0.375～9mg mL-1。
Described step 2) in, the compactedness of described water heating kettle controls 10～80%.
Described CNTs is selected from carboxylated multi-walled carbon nano-tubes, and internal diameter is 5～15nm, and external diameter is 20～100nm, and length is 10～30 μm.
Described SnO2SnO in/CNTs combination electrode material2Particle diameter be 5nm, SnO2It is grown in the surface of CNTs.
Beneficial effects of the present invention is embodied in:
The present invention is using water as solvent, with SnCl2·2H2O, as Xi Yuan, adopts one step hydro thermal method to be prepared for SnO2Particle diameter is the SnO of 5nm2/ CNTs composite, and SnO2The evengranular surface being grown in CNTs.The preparation method that the present invention uses is simple, and repeatability is high, reaction temperature is low, the cycle is short, energy consumption is low, needs prepared by applicable large-scale production, has significant scientific meaning in sodium-ion battery application aspect.
Accompanying drawing explanation
Fig. 1 is the SnO prepared by embodiment 32X-ray diffraction (XRD) collection of illustrative plates of/CNTs composite；
Fig. 2 is the SnO prepared by embodiment 32Scanning electron microscope (SEM) photo of/CNTs composite；
Fig. 3 is the SnO prepared by embodiment 32Transmission electron microscope (TEM) photo of/CNTs composite.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is elaborated.
Embodiment 1
1) being added by 30mgCNTs in 50mL deionized water, after stirring, supersound process (50W) 100min obtains uniform mixed liquor A, and in mixed liquor A, the concentration of CNTs is 0.6mg mL-1；Then in mixed liquor A, add 0.5245gSnCl again2·2H2O, after stirring, supersound process (50W) 100min obtains uniform mixed liquid B.
2) mixed liquid B obtained above is transferred in politef water heating kettle, it is subsequently placed in homogeneous reactor (Yantai Ke Li Chemical Equipment Co., Ltd., KLJX-8A) in (compactedness controls 50%), reacting 12h at 120 DEG C, reaction naturally cools to room temperature after terminating.Then pass through the centrifugal powder body that will be obtained by reacting separation, the powder freezing that separation obtains is dried and obtains SnO2/ CNTs electrode material (SnO2/ CNTs complex powder body).
3) sample (SnO is analyzed with Rigaku D/max2000PCX-x ray diffractometer x2/ CNTs complex powder body), it has been found that sample and JCPDS are numbered the SnO of the tetragonal crystal system of 71-06522Structure is consistent, but does not have obvious carbon peak to occur, it may be possible to carbon at the peak of 26 ° by SnO2Peak herein is covered.This sample field emission scanning electron microscope (FESEM) of FEI Co. of U.S. S-4800 type is observed, it can be seen that prepared SnO2The evengranular surface being grown in CNTs；Observed by the Flied emission transmission electron microscope of FEI Co. of U.S. TecnaiG2F20S-TWIN type further, it can be seen that SnO2Particle diameter be approximately 5nm.
Embodiment 2
1) being added by 50mgCNTs in 50mL deionized water, after stirring, supersound process (60W) 120min obtains uniform mixed liquor A, and in mixed liquor A, the concentration of CNTs is 1mg mL-1；Then in mixed liquor A, add 0.32gSnCl again2·2H2O, after stirring, supersound process (60W) 120min obtains uniform mixed liquid B.
2) mixed liquid B obtained above is transferred in politef water heating kettle, it is subsequently placed in homogeneous reactor (Yantai Ke Li Chemical Equipment Co., Ltd., KLJX-8A) in (compactedness controls 50%), reacting 8h at 180 DEG C, reaction naturally cools to room temperature after terminating.Then pass through the centrifugal powder body that will be obtained by reacting separation, the powder freezing that separation obtains is dried and obtains SnO2/ CNTs electrode material (SnO2/ CNTs complex powder body).
3) sample (SnO is analyzed with Rigaku D/max2000PCX-x ray diffractometer x2/ CNTs complex powder body), it has been found that sample and JCPDS are numbered the SnO of the tetragonal crystal system of 71-06522Structure is consistent, but does not have obvious carbon peak to occur, it may be possible to carbon at the peak of 26 ° by SnO2Peak herein is covered.This sample field emission scanning electron microscope (FESEM) of FEI Co. of U.S. S-4800 type is observed, it can be seen that prepared SnO2The evengranular surface being grown in CNTs；Observed by the Flied emission transmission electron microscope of FEI Co. of U.S. TecnaiG2F20S-TWIN type further, it can be seen that SnO2Particle diameter be approximately 5nm.
Embodiment 3
1) being added by 50mgCNTs in 80mL deionized water, after stirring, supersound process (50W) 60min obtains uniform mixed liquor A, and in mixed liquor A, the concentration of CNTs is 0.625mg mL-1；Then in mixed liquor A, add 0.6765gSnCl again2·2H2O, after stirring, supersound process (50W) 60min obtains uniform mixed liquid B.
2) mixed liquid B obtained above is transferred in politef water heating kettle, it is subsequently placed in homogeneous reactor (Yantai Ke Li Chemical Equipment Co., Ltd., KLJX-8A) in (compactedness controls 80%), reacting 3h at 150 DEG C, reaction naturally cools to room temperature after terminating.Then pass through the centrifugal powder body that will be obtained by reacting separation, the powder freezing that separation obtains is dried and obtains SnO2/ CNTs electrode material (SnO2/ CNTs complex powder body).
3) sample (SnO is analyzed with Rigaku D/max2000PCX-x ray diffractometer x2/ CNTs complex powder body), it has been found that sample and JCPDS are numbered the SnO of the tetragonal crystal system of 71-06522Structure is consistent, but does not have obvious carbon peak to occur, it may be possible to carbon at the peak of 26 ° by SnO2(Fig. 1) is covered at peak herein.This sample field emission scanning electron microscope (FESEM) of FEI Co. of U.S. S-4800 type is observed, it can be seen that prepared SnO2The evengranular surface (Fig. 2) being grown in CNTs；Observed by the Flied emission transmission electron microscope of FEI Co. of U.S. TecnaiG2F20S-TWIN type further, it can be seen that SnO2Particle diameter be approximately 5nm (Fig. 3).
Embodiment 4
1) being added by 80mgCNTs in 80mL deionized water, after stirring, supersound process (100W) 120min obtains uniform mixed liquor A, and in mixed liquor A, the concentration of CNTs is 1mg mL-1；Then in mixed liquor A, add 1.353gSnCl again2·2H2O, after stirring, supersound process (100W) 120min obtains uniform mixed liquid B.
2) mixed liquid B obtained above is transferred in politef water heating kettle, it is subsequently placed in homogeneous reactor (Yantai Ke Li Chemical Equipment Co., Ltd., KLJX-8A) in (compactedness controls 80%), reacting 3h at 210 DEG C, reaction naturally cools to room temperature after terminating.Then pass through the centrifugal powder body that will be obtained by reacting separation, the powder freezing that separation obtains is dried and obtains SnO2/ CNTs electrode material (SnO2/ CNTs complex powder body).
3) sample (SnO is analyzed with Rigaku D/max2000PCX-x ray diffractometer x2/ CNTs complex powder body), it has been found that sample and JCPDS are numbered the SnO of the tetragonal crystal system of 71-06522Structure is consistent, but does not have obvious carbon peak to occur, it may be possible to carbon at the peak of 26 ° by SnO2Peak herein is covered.This sample field emission scanning electron microscope (FESEM) of FEI Co. of U.S. S-4800 type is observed, it can be seen that prepared SnO2The evengranular surface being grown in CNTs；Observed by the Flied emission transmission electron microscope of FEI Co. of U.S. TecnaiG2F20S-TWIN type further, it can be seen that SnO2Particle diameter be approximately 5nm.
Embodiment 5
1) being added by 50mgCNTs in 30mL deionized water, after stirring, supersound process (100W) 120min obtains uniform mixed liquor A, and in mixed liquor A, the concentration of CNTs is 1.67mg mL-1；Then in mixed liquor A, add 0.5245gSnCl again2·2H2O, after stirring, supersound process (100W) 120min obtains uniform mixed liquid B.
2) mixed liquid B obtained above is transferred in politef water heating kettle, it is subsequently placed in homogeneous reactor (Yantai Ke Li Chemical Equipment Co., Ltd., KLJX-8A) in (compactedness controls 30%), reacting 12h at 150 DEG C, reaction naturally cools to room temperature after terminating.Then pass through the centrifugal powder body that will be obtained by reacting separation, the powder freezing that separation obtains is dried and obtains SnO2/ CNTs electrode material (SnO2/ CNTs complex powder body).
3) sample (SnO is analyzed with Rigaku D/max2000PCX-x ray diffractometer x2/ CNTs complex powder body), it has been found that sample and JCPDS are numbered the SnO of the tetragonal crystal system of 71-06522Structure is consistent, but does not have obvious carbon peak to occur, it may be possible to carbon at the peak of 26 ° by SnO2Peak herein is covered.This sample field emission scanning electron microscope (FESEM) of FEI Co. of U.S. S-4800 type is observed, it can be seen that prepared SnO2The evengranular surface being grown in CNTs；Observed by the Flied emission transmission electron microscope of FEI Co. of U.S. TecnaiG2F20S-TWIN type further, it can be seen that SnO2Particle diameter be approximately 5nm.
In above-described embodiment 1～5, CNTs is selected from carboxylated multi-walled carbon nano-tubes TNM5 (internal diameter is 5～10nm, and external diameter is 20～30nm, and length is 10～30 μm), and carboxylated multi-walled carbon nano-tubes, except TNM5, also includes TNM7, TNM8.
In a word, the present invention, using water as solvent, adopts one step hydro thermal method to be prepared for SnO2/ CNTs composite, owing in this composite, CNTs has good structural stability, higher conductivity and SnO2For nano-scale particle, therefore, using it as anode material of lithium-ion battery, there is the chemical property (such as, higher capacity, have good cyclical stability and high rate performance) of excellence；The preparation method that the present invention uses is simple, and reaction temperature is low, the cycle is short, energy consumption is low, therefore has very big scientific meaning in sodium-ion battery application aspect.
Claims (6)
1. a sodium-ion battery negative pole SnO2The preparation method of/CNTs combination electrode material, it is characterised in that: comprise the following steps:
1) being added in 10～80mL deionized water by 30～90mgCNTs, after stirring, supersound process 10～120min obtains mixed liquor A；Then in described mixed liquor A, add 0.1～2.706gSnCl again2·2H2O, after stirring, supersound process 10～120min obtains mixed liquid B；
2) described mixed liquid B is transferred in politef water heating kettle, then politef water heating kettle it is placed in homogeneous reactor and at 120～230 DEG C, reacts 2～50h, reaction is cooled to room temperature after terminating, then pass through the centrifugal powder body that will be obtained by reacting separation, the powder freezing that separation obtains is dried and obtains SnO2/ CNTs combination electrode material.
2. a kind of sodium-ion battery negative pole SnO according to claim 12The preparation method of/CNTs combination electrode material, it is characterised in that: described step 1) in, SnCl2·2H2The mass ratio of O and CNTs is 4.3～90.2:1.
3. a kind of sodium-ion battery negative pole SnO according to claim 12The preparation method of/CNTs combination electrode material, it is characterised in that: in described mixed liquor A, the concentration of CNTs is 0.375～9mg mL-1。
4. a kind of sodium-ion battery negative pole SnO according to claim 12The preparation method of/CNTs combination electrode material, it is characterised in that: described step 2) in, the compactedness of described water heating kettle controls 10～80%.
5. a kind of sodium-ion battery negative pole SnO according to claim 12The preparation method of/CNTs combination electrode material, it is characterised in that: described CNTs is selected from carboxylated multi-walled carbon nano-tubes, and the internal diameter of multi-walled carbon nano-tubes is 5～15nm, and external diameter is 20～100nm, and length is 10～30 μm.
6. a kind of sodium-ion battery negative pole SnO according to claim 12The preparation method of/CNTs combination electrode material, it is characterised in that: described SnO2SnO in/CNTs combination electrode material2Particle diameter be 5nm, SnO2It is grown in the surface of CNTs.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106058198A (en) * | 2016-07-26 | 2016-10-26 | 陕西科技大学 | Method for preparing SnS2/CNTs (carbon nano-tubes) cathode materials for sodium-ion batteries in in-situ manner |
| CN106602035A (en) * | 2017-01-13 | 2017-04-26 | 陕西科技大学 | Preparation method of compound powder with tubular biochar-coated SnO<2> structure and application of compound powder |
| CN106848279A (en) * | 2017-01-13 | 2017-06-13 | 陕西科技大学 | A kind of liquid phase adsorbs SnO certainly2The preparation method and application of/biological carbon composite |
| CN107176590A (en) * | 2017-05-08 | 2017-09-19 | 太原理工大学 | Highly controllable ternary heterojunction structure material of constituent content and preparation method thereof |
| CN108461726A (en) * | 2018-03-12 | 2018-08-28 | 陕西科技大学 | A kind of polycrystalline manganese dioxide/carbon nanotube composite material and its preparation method and application |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106058198A (en) * | 2016-07-26 | 2016-10-26 | 陕西科技大学 | Method for preparing SnS2/CNTs (carbon nano-tubes) cathode materials for sodium-ion batteries in in-situ manner |
| CN106602035A (en) * | 2017-01-13 | 2017-04-26 | 陕西科技大学 | Preparation method of compound powder with tubular biochar-coated SnO<2> structure and application of compound powder |
| CN106848279A (en) * | 2017-01-13 | 2017-06-13 | 陕西科技大学 | A kind of liquid phase adsorbs SnO certainly2The preparation method and application of/biological carbon composite |
| CN106602035B (en) * | 2017-01-13 | 2019-02-26 | 陕西科技大学 | A kind of tubulose biology carbon coating SnO2Structure composite raw powder's production technology and application |
| CN106848279B (en) * | 2017-01-13 | 2019-08-09 | 陕西科技大学 | A kind of liquid phase is from adsorbing SnO2The preparation method and application of/biology carbon composite |
| CN107176590A (en) * | 2017-05-08 | 2017-09-19 | 太原理工大学 | Highly controllable ternary heterojunction structure material of constituent content and preparation method thereof |
| CN108461726A (en) * | 2018-03-12 | 2018-08-28 | 陕西科技大学 | A kind of polycrystalline manganese dioxide/carbon nanotube composite material and its preparation method and application |
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