CN103303968B - A kind of CdSnO 3nano material and its preparation method and application - Google Patents
A kind of CdSnO 3nano material and its preparation method and application Download PDFInfo
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- CN103303968B CN103303968B CN201310155725.3A CN201310155725A CN103303968B CN 103303968 B CN103303968 B CN 103303968B CN 201310155725 A CN201310155725 A CN 201310155725A CN 103303968 B CN103303968 B CN 103303968B
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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
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a kind of CdSnO
3nano material and its preparation method and application, comprises the following steps: first adopt hydro thermal method to prepare poroid CdSn (OH)
6presoma; Then the poroid CdSn (OH) will obtained
6nano particle is calcined, and can obtain highly mesoporous CdSnO
3nano particle.The CdSnO obtained by the inventive method
3nanometer anode material, its pore diameter range is approximately 7.8nm ~ 28.7nm, shows higher specific capacity, good high rate performance and cyclical stability, can be used for the negative material of high performance lithium ion battery of future generation, have broad application prospects; And preparation method of the present invention is without the need to special installation and harsh conditions, technique is simple, and controllability is strong, abundant raw materials and cheap, easily realizes large-scale production, has very strong practicality.
Description
Technical field
The invention belongs to novel energy resource material technology field, more precisely, relate to a kind of CdSnO
3nano material, the invention still further relates to this CdSnO
3the preparation of nano material and application thereof.
Background technology
Lithium ion battery, as portable electric appts (mobile phone, digital camera etc.) topmost dynamic origin, has obtained and has studied widely.Although graphite cathode is commercialization, its relatively low theoretical capacity (372mAhg
-1) can not meet the demand of future market, therefore at present still in the urgent need to developing the Novel cathode material for lithium ion battery that some have height ratio capacity and high power density.The capacity that can provide due to tin-based composites be the 2-3 of graphite capacity doubly, be therefore regarded as the negative material of very promising novel high-performance lithium ion battery.In addition, tin-based composites has a relatively low intercalation potential (about 0.5V), and this shows that tin-based composites is very suitable for lithium ion battery negative material further.Unfortunately tin base cathode material is in charge and discharge process, due to the embedding/deviate from process to cause huge change in volume at Li+, causes the capacity fade problem faced in its cyclic process sharply, which has limited their application in practice.In order to improve or solve the problem of its capacity attenuation, invent a simple effective method and go the various novel nanostructure of design and synthesis to be the key addressed this problem.
In the past few decades, as the CdSnO of tin-based composites material representative
3mainly studied as gas sensitive.But, as far as we know for CdSnO
3the report that material is used as lithium ion battery material is very limited.
Summary of the invention
The present invention, in order to solve problems of the prior art, prepares the negative material of porous nanometer structure to improve its energy and power density method by research, provides a kind of CdSnO
3nano material, the hole that this material exists partly can cushion Li+ and repeatedly embed/deviate from the volumetric expansion caused, to prevent capacity attenuation.
In order to realize above-mentioned object, technical scheme of the present invention is: a kind of CdSnO
3nano material, described CdSnO
3have highdensity mesoporous in the particle diameter of nano material.
Present invention also offers one and prepare above-mentioned CdSnO
3the method of nano material, comprises the following steps:
A) butter of tin, chromium chloride, citric acid are dissolved in the water environment of alkalescence, obtain mixed liquor;
B) by step a) in mixed liquor to pour in reactor heating into and react, obtain presoma CdSn (OH)
6mixed liquor;
C) by step b) CdSn (OH) that obtains
6mixed liquor, through washing, centrifugal after dry in solid;
D) by step c) in the drying solid that obtains calcine, obtain that there is the mesoporous CdSnO of high density
3nano material.
Preferably, described step a) in alkaline aqueous environment be sodium hydrate aqueous solution.
Preferably, described step b) in reaction temperature be 160-200 DEG C.
Preferably, described steps d) in calcine in Muffle furnace.
Preferably, the temperature of calcining is 500-600 DEG C.
Preferably, the temperature of described calcining is 550 DEG C, and the time of calcining is 6 hours.
The present invention also protects this CdSnO
3the application of nano material in cell negative electrode material.
The present invention also protects this CdSnO
3the application of nano material in light-sensitive material.
Compared with prior art, the present invention has following beneficial effect:
1) CdSnO that the height prepared of reason the inventive method is mesoporous
3nanometer negative materials for Li-ion batteries, its pore diameter range is approximately 7.8nm ~ 28.7nm, and the existence of this some holes can provide large pore volume, effectively adds active material CdSnO on the one hand
3and the contact area between electrolyte, is conducive to Li
+transmission; Be conducive on the other hand cushioning Li
+the volumetric expansion caused in embedding/deintercalation process, maintains the stability of its structure in charge and discharge process, finally makes it show high specific capacity and high rate performance ((70mAhg
-1, 515mAhg
-1); (150mAhg
-1, 506mAhg
-1)).
2) preparation method of the present invention is without the need to special installation and harsh conditions, and synthetic method is simple, can synthesize in enormous quantities, have practicality.
Accompanying drawing explanation
Fig. 1 is the presoma CdSn (OH) for the embodiment of the present invention 1 provides
6highly mesoporous CdSnO
3xRD diffraction pattern;
Fig. 2 is the CdSn (OH) of the presoma provided for the embodiment of the present invention 1
6transmission electron microscope photo;
Fig. 3 is the mesoporous CdSnO of the height that provides for the embodiment of the present invention 1
3transmission electron microscope photo;
Fig. 4 a-Fig. 4 c is the mesoporous CdSnO of height that the embodiment of the present invention 1 provides
3electrochemical property test result.In figure: Fig. 4 a represents the mesoporous CdSnO that embodiment 1 obtains
3charging and discharging curve (the measuring current 70mAhg that nano-electrode is representative
-1), Fig. 4 b represents its cycle performance curve (measuring current 70mAhg
-1), Fig. 4 c represents that (measuring current is followed successively by 60mAhg to its circulation performance curve
-1, 90mAhg
-1, 120mAhg
-1, 150mAhg
-1).
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, do to illustrate in detail, intactly further to the present invention below in conjunction with embodiment and accompanying drawing.
Set forth a lot of detail in the following description so that fully understand the present invention, but the present invention can also adopt other to be different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar popularization when intension of the present invention, therefore the present invention is by the restriction of following public specific embodiment.
Material in the embodiment of the present invention all can commercially buy.By following simple, effective method, the mesoporous CdSnO of high density successfully can be synthesized in enormous quantities
3nano material, its pore diameter range is approximately 7.8nm ~ 28.7nm.By showing the CdSnO that the height of acquisition is mesoporous to sample electrode electrochemical property test result
3nanometer anode material shows high reversible capacity, good high rate performance and cyclical stability.Wherein at current density 70mAhg
-1it is approximately 515mAhg that lower charge and discharge cycles 40 encloses rear capacity
-1, and when current density is increased to 150mAhg
-1time, capacity still remains on 506mAhg
-1.
Embodiment 1
Respectively by 0.228gCdCl
22.5H
2o and 0.21g citric acid is dissolved in 10mL water, and 0.351gSnCl
45H
2o is dissolved in 5mL water.Then by after two kinds of solution mixing, then add 0.40gNaOH and 25mL water, obtain final mixed liquor.Then the mixed liquor of 40mL is poured in the hydrothermal reaction kettle of 60mL, put into baking oven and keep 180 DEG C and react 12h, obtain presoma CdSn (OH)
6mixed liquor.
By the presoma CdSn (OH) obtained
6the mixed solution washing of sample deionized water and ethanol, 60 DEG C of oven dry after centrifugal, obtains CdSn (OH)
6white solid powder;
CdSn (OH) will be obtained
6white solid powder, to be placed in Muffle furnace 550 DEG C of calcining 6h, to obtain highly mesoporous CdSnO
3nanometer anode material.
The stoichiometric proportion of above-mentioned each material can be allocated according to the cognition of those skilled in the art, it finally can generate final product, washing, centrifugal means are ordinary skill in the art means, dry temperature and time does not limit, it can be at air drying, can also carry out heat drying.The selection of above-mentioned each parameter, can choose, such as calcining heat 550 DEG C, can select in the valid interval of 500-600 DEG C in the valid interval of above-mentioned concrete numerical value, and differing at this one illustrates.
Fig. 1 is the presoma CdSn (OH) that the present embodiment obtains
6highly mesoporous CdSnO
3xRD diffraction pattern, known through XRD interpretation of result: the CdSn (OH) obtained
6the CdSnO mesoporous with high density
3nanometer anode material can index be the CdSn (OH) of Emission in Cubic respectively
6and the CdSnO of orthorhombic phase (JCPDSNo.28-0202)
3(JCPDSNo.34-0758R-3 (148)).
Fig. 2 is the presoma CdSn (OH) that the present embodiment obtains
6transmission electron microscope photo, as seen from Figure 2: the CdSn (OH) obtained
6nano particle average-size is about 70nm.
Fig. 3 is that the present embodiment obtains the mesoporous CdSnO of the height that provides
3transmission electron microscope photo.As seen from Figure 3: the mesoporous CdSnO obtained
3its pore diameter range of nano particle is approximately 7.8nm ~ 28.7nm.
According to the characteristic of above-mentioned experimental data and material itself, this mesoporous CdSnO
3nano particle can be applicable in light-sensitive material.The present invention prepares the chemical property of sample in order to research institute, and the electro-chemical test of product adopts No. 2016 button cell analog detection of the two poles of the earth system.Using the pour lithium slice of same diameter as positive electrode, capillary polypropylene (Celgard-2400) as barrier film, 1.0molL
-1liPF
6ethyl carbonate (EC) and the mixed solution (volume ratio is 1:1) of diethyl carbonate (DEC) as electrolyte.The assembling process of battery is carried out in the glove box being full of high-purity argon gas.Electrochemical properties LAND-CT2001A tests, and detects within the scope of the charging/discharging voltage of 0.005-1V to the charge/discharge capacity of battery, circulation and high rate performance.
Testing result shows: highly mesoporous CdSnO
3nanometer anode material illustrates good high rate performance and cyclical stability.
Fig. 4 is the mesoporous CdSnO of height that the present embodiment obtains
3electrochemical property test result.In figure: a represents the mesoporous CdSnO that embodiment 1 obtains
3charging and discharging curve (the current density 70mAhg that nano-electrode is representative
-1), b represents its cycle performance curve (measuring current 70mAhg
-1), c represents that (measuring current is followed successively by 60mAhg to its circulation performance curve
-1, 90mAhg
-1, 120mAhg
-1, 150mAhg
-1).From Fig. 4 a-Fig. 4 c: this material is 70mAhg in current density
-1lower charge and discharge cycles 40 is enclosed rear capacity and is kept being approximately 515mAhg
-1, and when current density is increased to 150mAhg
-1time, capacity still keeps 506mAhg
-1, the high rate performance shown and cyclical stability.
Embodiment 2
The difference of the present embodiment and embodiment 1 is only: in step a) not adding citric acid, all the other contents are all identical with described in embodiment 1.
Analyze after testing and learn: the mesoporous CdSnO that the present embodiment obtains
3nanometer anode material size distribution ranges is wide, and has serious gathering situation to occur.
The mesoporous CdSnO that the present embodiment obtains
3nanometer anode material with the test performance obviously ((70mAhg far short of what is expected that obtains under embodiment 1 the same terms
-1, 340mAhg
-1); (150mAhg
-1, 173mAhg
-1)).
Visible in sum: can to obtain by the inventive method the orthorhombic phase CdSnO that a kind of average grain diameter is approximately 50nm
3nano particle, and its pore diameter range is 7.8nm ~ 28.7nm, and it is mesoporous to have high density, the mesoporous of this material existence partly can cushion Li
+repeatedly embed/deviate from the volumetric expansion caused, to prevent capacity attenuation.Improve its reversible capacity, and the high rate performance shown and cyclical stability, there is application prospect; And described preparation method is without the need to special installation and harsh conditions, simple, controllability is strong, easily accomplishes scale production, has practicality.
Finally be necessary described herein: above embodiment is only for being described in more detail technical scheme of the present invention; can not be interpreted as limiting the scope of the invention, some improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention.
Claims (1)
1. prepare CdSnO for one kind
3the method of nano material, is characterized in that: comprise the following steps:
A) be 0.228gCdCl by quality respectively
22.5H
2o and 0.21g citric acid is dissolved in 10mL water, and 0.351gSnCl
45H
2o is dissolved in 5mL water, adds 0.40gNaOH and 25mL water again, obtain mixed liquor after mixing;
B) by step a) in mixed liquor pour in reactor and react 12h at 180 DEG C, obtain presoma CdSn (OH)
6mixed liquor;
C) by step b) CdSn (OH) that obtains
6mixed liquor, through washing, centrifugal after 60 DEG C of dryings be solid;
D) by step c) in the drying solid that obtains at 550 DEG C, calcine 6h, obtain that there is the mesoporous CdSnO of high density
3nano material.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310155725.3A CN103303968B (en) | 2013-04-28 | 2013-04-28 | A kind of CdSnO 3nano material and its preparation method and application |
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|---|---|---|---|
| CN201310155725.3A CN103303968B (en) | 2013-04-28 | 2013-04-28 | A kind of CdSnO 3nano material and its preparation method and application |
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|---|---|
| CN103303968A CN103303968A (en) | 2013-09-18 |
| CN103303968B true CN103303968B (en) | 2015-11-25 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111239205A (en) * | 2020-01-30 | 2020-06-05 | 吉林大学 | Based on CdSnO3Isopropyl alcohol gas sensor of sensitive layer and preparation method thereof |
| CN113371754B (en) * | 2021-06-23 | 2022-06-10 | 石久光学科技发展(北京)有限公司 | High-purity cadmium stannate powder and preparation method thereof |
| CN116565042B (en) * | 2023-07-12 | 2023-09-22 | 长春理工大学 | Preparation method of self-assembled tin oxide and cadmium oxide nanostructure superlattice |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101442116A (en) * | 2008-12-18 | 2009-05-27 | 宁波职业技术学院 | Preparation method for lithium ion battery amorphous state tin plumbum composite oxide cathode material |
| CN102983318A (en) * | 2012-12-12 | 2013-03-20 | 苏州大学 | Material for negative electrode of non-aqueous secondary battery, preparation method of material, non-aqueous secondary battery and negative electrode thereof |
-
2013
- 2013-04-28 CN CN201310155725.3A patent/CN103303968B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101442116A (en) * | 2008-12-18 | 2009-05-27 | 宁波职业技术学院 | Preparation method for lithium ion battery amorphous state tin plumbum composite oxide cathode material |
| CN102983318A (en) * | 2012-12-12 | 2013-03-20 | 苏州大学 | Material for negative electrode of non-aqueous secondary battery, preparation method of material, non-aqueous secondary battery and negative electrode thereof |
Non-Patent Citations (3)
| Title |
|---|
| Lithium-storage and cycleability of nano-CdSnO3 as an anode material for lithium-ion batteries;Yogesh Sharma et al.;《Journal of Power Sources》;20090327;第192卷;627-635 * |
| Mesoporous Single-crystal CoSn(OH)6 Hollow Structures with Multilevel Interiors;Zhiyu Wang et al.;《SCIENTIFIC REPORTS》;20130306;第3卷;1391-1398 * |
| Photoelectrochemical Study of the Ilmenite Polymorph of CdSnO3 and Its Photoanodic Application in Dye-Sensitized Solar Cells;Gayatri Natu et al.;《J. Phys. Chem. C》;20100403;第114卷;6802-6807 * |
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