CN105514404B - A kind of spherical SnO of nano particle assembling burr2Anode material of lithium-ion battery and preparation method thereof - Google Patents
A kind of spherical SnO of nano particle assembling burr2Anode material of lithium-ion battery and preparation method thereof Download PDFInfo
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- CN105514404B CN105514404B CN201610049012.2A CN201610049012A CN105514404B CN 105514404 B CN105514404 B CN 105514404B CN 201610049012 A CN201610049012 A CN 201610049012A CN 105514404 B CN105514404 B CN 105514404B
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- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 30
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 30
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000463 material Substances 0.000 title claims description 9
- 239000010405 anode material Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 15
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000012456 homogeneous solution Substances 0.000 claims abstract description 6
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims abstract description 6
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 3
- 229910001415 sodium ion Inorganic materials 0.000 claims description 9
- 238000007710 freezing Methods 0.000 claims description 6
- 230000008014 freezing Effects 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims 3
- 239000010406 cathode material Substances 0.000 claims 1
- 238000004108 freeze drying Methods 0.000 abstract description 3
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 11
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 7
- 239000002245 particle Substances 0.000 description 4
- 230000002441 reversible effect Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
Classifications
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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
-
- 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
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
The present invention discloses a kind of spherical SnO of nano particle assembling burr2Anode material of lithium-ion battery and preparation method thereof, including：1) by SnCl4·5H2O and CO (NH2)2It is dissolved in aliquots of deionized water respectively, is configured to solution A and solution B；2) B solution is slowly added to solution A under continuing magnetic force stirring action and forms homogeneous solution C, N is added dropwise into solution CaOH solution Es form solution D；3) homogeneous hydro-thermal reaction is carried out；4) it waits for after reaction, taking out presoma, washing obtains white presoma, and freeze-drying obtains the spherical SnO of nano particle assembling burr2Anode material of lithium-ion battery.Preparation method of the present invention is at low cost, easy to operate, short preparation period；The spherical SnO of prepared nano particle assembling burr2Anode material of lithium-ion battery charge-discharge performance is excellent, and under the current density of 50mA/g, discharge capacity can reach 1400mAh/g for the first time, has higher capacity and cyclical stability under high current density.
Description
Technical field
The present invention relates to sodium-ion battery technical field, more particularly to a kind of anode material of lithium-ion battery and its preparation side
Method.
Background technology
Sodium-ion battery is a kind of model electrochemical power supply, has that raw material resources are abundant, cost is relatively low, specific capacity and effect
The advantages that rate is higher more meets the requirement of scale stored energy application, is promoting extensive regenerative resource grid integration ability, is carrying
There is application potential, simultaneously because its specific capacity height, light weight, long lifespan and nothing in terms of high electric energy service efficiency and power quality
The significant advantages such as Memorability also have extensive in fields such as aerospace, hybrid-electric car and portable electronic devices
Using.In this context, sodium-ion battery causes the extensive concern in worldwide, critical material and related skill in recent years
Art progress is rapid.But for opposite lithium ion, sodium ion has larger ionic radius (0.102nm vs.0.076nm
Of Li), this so that finding suitable embedding sodium material tool acquires a certain degree of difficulty.
Invention content
The purpose of the present invention is to provide a kind of spherical SnO of nano particle assembling burr2Anode material of lithium-ion battery and
Preparation method, manufacturing cost is low, easy to operate, short preparation period, and the particle of acquisition assembles spherical SnO2Sodium-ion battery
Negative material is had excellent performance.
To achieve the goals above, the present invention adopts the following technical scheme that：
A kind of spherical SnO of nano particle assembling burr2The preparation method of anode material of lithium-ion battery, including following step
Suddenly：
1) by SnCl4·5H2O and CO (NH2)2It is dissolved in aliquots of deionized water respectively, is configured to solution A and solution B；Its
In, m in mass ratioSnCl4·5H2O：mCO(NH2)2=1:0.4~1:1.5；
2) B solution is slowly added to solution A under continuing magnetic force stirring action and forms homogeneous solution C, dropwise into solution C
N is addedaOH solution Es form solution D；The volume of solution C and the volume ratio of solution E are 5:2~3:4；
3) it waits for after reaction, solution D being put into hydrothermal reaction kettle and is sealed, carries out homogeneous hydro-thermal reaction；
4) it waits for after reaction, taking out presoma, washing obtains white presoma, and freeze-drying obtains nano particle assembling
The spherical SnO of burr2Anode material of lithium-ion battery.
Further, in solution A Sn a concentration of 0.5~1.2mol/L.
Further, NaThe solubility of OH solution Es is 0.3~1.4mol/L.
Further, the condition of homogeneous hydro-thermal reaction is：At 80~220 DEG C, the reaction time controls 8 for reaction temperature control
~48h.
Further, the washing is specially to distinguish centrifuge washing 2~3 times through deionized water and absolute ethyl alcohol.
Further, the freeze-drying is specially that prepared presoma is subzero in the freezing chamber of freeze drier
50-60 DEG C of freezing 4-5h, then dries 10-12h at room temperature in vacuum drying cabinet.
A kind of spherical SnO of nano particle assembling burr2The preparation method of anode material of lithium-ion battery, prepared nanometer
Particle assembles the spherical SnO of burr2Anode material of lithium-ion battery.
Compared with the existing technology, the invention has the advantages that：
Preparation method of the present invention is at low cost, easy to operate, short preparation period；Prepared nano particle assembling burr is spherical
SnO2Anode material of lithium-ion battery particle size only has a few to tens of nanometers, and assembling ball size is about 300~400nm, purity
Height, crystallinity is strong, pattern is uniform, is applied to sodium-ion battery cathode, and charge-discharge performance is excellent, close in the electric current of 50mA/g
Under degree, discharge capacity can reach 1400mAh/g for the first time, have higher capacity and cyclical stability under high current density.
Description of the drawings
Fig. 1 is the spherical SnO of nano particle assembling burr prepared by example 1 of the present invention2The SEM of anode material of lithium-ion battery
Figure.
Fig. 2 is the spherical SnO of nano particle assembling burr prepared by example 1 of the present invention2Anode material of lithium-ion battery electrification
Learn performance map.
Specific implementation mode
Embodiment 1
A kind of spherical SnO of nano particle assembling burr2The preparation method of anode material of lithium-ion battery, including following step
Suddenly：
1) by SnCl4·5H2O is dissolved in deionized water, is configured to the solution A of a concentration of 0.5mol/L；In mass ratio
mSnCl4·5H2O： mCO(NH2)2=1:0.4 by urea (CO (NH2)2) be added in aliquots of deionized water, it is configured to solution B；
2) B solution is slowly added to solution A under continuing magnetic force stirring action and forms homogeneous solution C, dropwise into solution C
0.3mol/L N are addedaOH solution Es form solution D, persistently stir 0.5h afterwards；The volume of solution C and the volume ratio of solution E are
5:2；
3) it waits for after reaction, solution D being put into hydrothermal reaction kettle and is sealed, is put into homogeneous hydro-thermal reaction instrument, reaction temperature
At 80 DEG C, the reaction time controls in 8h for degree control；
4) it waits for after reaction, taking out presoma, distinguishes centrifuge washing 2 times through deionized water and absolute ethyl alcohol, obtain white
Color presoma, subzero 50 DEG C of the freezing chamber by prepared presoma in freeze drier freezes 5h, then in vacuum drying cabinet
10h is dried at room temperature obtains the spherical SnO of nano particle assembling burr2Anode material of lithium-ion battery.
Fig. 1 is the spherical SnO of nano particle assembling burr prepared by the embodiment of the present invention 12Anode material of lithium-ion battery
SEM figure.As can be seen from the figure the surface of sample is that the burr that is assembled by nano particle is spherical, and nanoparticle size is about
It it is several nanometers, the grain size for assembling acanthosphere is about 150~180nm.Fig. 2 is the nano particle assembling prepared by the embodiment of the present invention 1
The spherical SnO of burr2Anode material of lithium-ion battery chemical property figure.As can be seen from the figure prepared nano particle assembles hair
Acanthosphere shape SnO2Anode material of lithium-ion battery, under the current density of 50mA/g, discharge capacity can reach for the first time
1400mAh/g has higher capacity and cyclical stability under high current density.
Embodiment 2
A kind of spherical SnO of nano particle assembling burr2The preparation method of anode material of lithium-ion battery, including following step
Suddenly：
1) by SnCl4·5H2O is dissolved in deionized water, is configured to the solution A of a concentration of 0.8mol/L；In mass ratio
mSnCl4·5H2O： mCO(NH2)2=1:0.9 by urea (CO (NH2)2) be added in aliquots of deionized water, it is configured to solution B；
2) B solution is slowly added to solution A under continuing magnetic force stirring action and forms homogeneous solution C, dropwise into solution C
0.8mol/L N are addedaOH solution Es form solution D, persistently stir 1h afterwards；The volume of solution C and the volume ratio of solution E are 4:
3；
3) it waits for after reaction, solution D being put into hydrothermal reaction kettle and is sealed, is put into homogeneous hydro-thermal reaction instrument, reaction temperature
At 150 DEG C, the reaction time controls in 36h for degree control；
4) it waits for after reaction, taking out presoma, distinguishes centrifuge washing 3 times through deionized water and absolute ethyl alcohol, obtain white
Color presoma, subzero 60 DEG C of the freezing chamber by prepared presoma in freeze drier freezes 4h, then in vacuum drying cabinet
11h is dried at room temperature obtains the spherical SnO of nano particle assembling burr2Anode material of lithium-ion battery.
Embodiment 3
A kind of spherical SnO of nano particle assembling burr2The preparation method of anode material of lithium-ion battery, including following step
Suddenly：
1) by SnCl4·5H2O is dissolved in deionized water, is configured to the solution A of a concentration of 1.2mol/L；In mass ratio
mSnCl4·5H2O： mCO(NH2)2=1:1.5 by urea (CO (NH2)2) be added in aliquots of deionized water, it is configured to solution B；
2) B solution is slowly added to solution A under continuing magnetic force stirring action and forms homogeneous solution C, dropwise into solution C
1.4mol/L N are addedaOH solution Es form solution D, persistently stir 2h afterwards；The volume of solution C and the volume ratio of solution E are 3:
4；
3) it waits for after reaction, solution D being put into hydrothermal reaction kettle and is sealed, is put into homogeneous hydro-thermal reaction instrument, reaction temperature
At 220 DEG C, the reaction time controls in 48h for degree control；
4) it waits for after reaction, taking out presoma, distinguishes centrifuge washing 3 times through deionized water and absolute ethyl alcohol, obtain white
Color presoma, subzero 50 DEG C of the freezing chamber by prepared presoma in freeze drier freezes 4h, then in vacuum drying cabinet
12h is dried at room temperature obtains the spherical SnO of nano particle assembling burr2Anode material of lithium-ion battery.
Stannic oxide also known as tin oxide, chemical formula SnO2, belong to group IV-VI Binary compound semiconductor, powder presents white
Color or yellow, 1127 DEG C of molten point, boiling point are higher than 190 DEG C, theoretical density 6.95g/cm3, belong to amphoteric oxide, dissolve in
Strong acid and highly basic.Cell parameter a=0.4738nm, b=0.4738mn, c=3.187nm, O2-Ionic radius 0.14nm, Sn4+From
Sub- radius 0.072nm, interior each structure cell includes two SnO2Molecule.Recent studies indicate that SnO2Nano material photocatalysis,
Gas sensor, transistor, Li-Ion rechargeable battery and solar cell etc. all have stronger application prospect, are considered
It is one of the semiconductor nano material for most having application prospect.SnO2The electrode material of base has big (the theoretical reversible appearance of embedding lithium capacity
Measure 781mAhg-1), good cycle, it is forthright good again the advantages that, theoretical reversible capacity is high, and practical reversible capacity is also remote
More than the theoretical reversible capacity of various lithium battery carbon negative pole materials commercial currently on the market.
Since granule-morphology may also can affect to the chemical property of sample, particle is smaller, specific surface
Product is bigger, then contact of the material with electrolyte is better, Na+Migration distance can also shorten, be more advantageous to sodium-ion battery in this way
The promotion of negative material high rate performance.
Claims (2)
1. a kind of spherical SnO of nano particle assembling burr2The preparation method of anode material of lithium-ion battery, which is characterized in that including
Following steps：
1) by SnCl4·5H2O is dissolved in deionized water, is configured to the solution A of a concentration of 0.5mol/L；In mass ratio
mSnCl4·5H2O：mCO(NH2)2=1:0.4 urea is added in aliquots of deionized water, is configured to solution B；
2) B solution is slowly added to solution A under continuing magnetic force stirring action and forms homogeneous solution C, be added dropwise into solution C
0.3mol/L NaOH solution Es form solution D, persistently stir 0.5h afterwards；The volume of solution C and the volume ratio of solution E are 5:2；
3) it waits for after reaction, solution D being put into hydrothermal reaction kettle and is sealed, is put into homogeneous hydro-thermal reaction instrument, reaction temperature control
At 80 DEG C, the reaction time controls in 8h system；
4) it waits for after reaction, taking out presoma, centrifuge washing is distinguished 2 times through deionized water and absolute ethyl alcohol, before obtaining white
Body is driven, subzero 50 DEG C of the freezing chamber by prepared presoma in freeze drier freezes 5h, then in vacuum drying cabinet room temperature
Lower dry 10h obtains the spherical SnO of nano particle assembling burr2Anode material of lithium-ion battery；
The prepared spherical SnO of nano particle assembling burr2Anode material of lithium-ion battery is the burr ball assembled by nano particle
Shape, the grain size for assembling acanthosphere are 150~180nm；The spherical SnO of prepared nano particle assembling burr2Sodium-ion battery cathode material
Material, under the current density of 50mA/g, discharge capacity can reach 1400mAh/g for the first time.
2. a kind of spherical SnO of nano particle assembling burr described in claim 12The preparation method of anode material of lithium-ion battery,
The prepared spherical SnO of nano particle assembling burr2Anode material of lithium-ion battery.
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| CN108807907B (en) * | 2018-06-12 | 2021-06-08 | 陕西科技大学 | Method for preparing particle self-assembly spherical tin monoxide/tin dioxide sodium ion battery cathode material by one-step method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101263287B1 (en) * | 2006-12-01 | 2013-05-10 | 삼성코닝정밀소재 주식회사 | Method of manufacturing tin oxide powder |
| CN103864139A (en) * | 2014-02-18 | 2014-06-18 | 上海大学 | Preparation method of three-dimensional layered multilevel flower-shaped stannic oxide microsphere |
| CN104528808A (en) * | 2014-12-27 | 2015-04-22 | 陕西科技大学 | Preparation method of hollow tin dioxide microsphere |
| CN104876259A (en) * | 2015-05-07 | 2015-09-02 | 浙江大学 | Preparation method of open tin dioxide hollow spheres |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101263287B1 (en) * | 2006-12-01 | 2013-05-10 | 삼성코닝정밀소재 주식회사 | Method of manufacturing tin oxide powder |
| CN103864139A (en) * | 2014-02-18 | 2014-06-18 | 上海大学 | Preparation method of three-dimensional layered multilevel flower-shaped stannic oxide microsphere |
| CN104528808A (en) * | 2014-12-27 | 2015-04-22 | 陕西科技大学 | Preparation method of hollow tin dioxide microsphere |
| CN104876259A (en) * | 2015-05-07 | 2015-09-02 | 浙江大学 | Preparation method of open tin dioxide hollow spheres |
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Effective date of registration: 20240731 Address after: 810, 8th Floor, Building 10, Courtyard 1, Tianxing Street, Fangshan District, Beijing, 102400 Patentee after: Beijing Zhichanhui Technology Co.,Ltd. Country or region after: China Address before: No. 1, Weiyang District university garden, Xi'an, Shaanxi Province, Shaanxi Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY Country or region before: China |