CN109133172A - A kind of niobic acid tin nanometer sheet and preparation method thereof and preparing the application in lithium battery - Google Patents
A kind of niobic acid tin nanometer sheet and preparation method thereof and preparing the application in lithium battery Download PDFInfo
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- CN109133172A CN109133172A CN201811004710.6A CN201811004710A CN109133172A CN 109133172 A CN109133172 A CN 109133172A CN 201811004710 A CN201811004710 A CN 201811004710A CN 109133172 A CN109133172 A CN 109133172A
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- C01G33/00—Compounds of niobium
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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
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- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract
The invention discloses a kind of SnNb2O6Nanometer sheet and preparation method thereof and the application in lithium battery is being prepared, is belonging to material preparation and lithium ion battery material technical field.Utilize a certain amount of K8Nb6O19、SnCl2·2H2O and ethanol water pass through hydro-thermal reaction, after cooling, centrifugation, washing, drying, obtain SnNb2O6Nanometer sheet.By a certain amount of SnNb2O6After nanometer sheet, sodium carboxymethylcellulose and acetylene black mixed grinding, adds water to be configured to mixed slurry, be uniformly coated on copper sheet, the cathode as lithium ion battery.SnNb disclosed by the invention2O6The preparation method of nanometer sheet has many advantages, such as easy to operate, at low cost.Use SnNb made from this method2O6Nanometer sheet purity is high, crystal type are good, can largely synthesize.Use the SnNb2O6Lithium ion battery with higher specific capacity, good circulation performance and high rate performance of the nanometer sheet as cathode.
Description
Technical field
The invention belongs to material preparation and lithium ion battery material technical fields, and in particular to a kind of niobic acid tin (SnNb2O6)
Nanometer sheet and preparation method thereof and preparing the application in lithium battery.
Background technique
Lithium ion battery because have many advantages, such as height ratio capacity, high voltage, have extended cycle life, memory-less effect and pollution it is small,
The fields such as mobile electronic device, small portable power-equipment and national defense industry are had been widely used at present.Electrode material is
The important component of lithium ion battery, and determine the key factor of performance of lithium ion battery.Currently, the lithium ion of commercialization
Secondary cell negative electrode material is mainly graphite, but graphite intercalation potential and lithium metal are close, the lithium easy to form in charge and discharge process
Dendrite causes battery short circuit, to cause some potential safety problems.Therefore, the breakthrough of lithium ion battery overall target is realized,
Vital " bottleneck " is how to design and Development of Novel electrode material.
Summary of the invention
In order to overcome the problems of the above-mentioned prior art, the purpose of the present invention is to provide a kind of SnNb2O6Nanometer sheet and
Preparation method and preparing the application in lithium battery, SnNb provided by the invention2O6The preparation method of nanometer sheet has operation
The advantages that easy, raw material is easy to get, is at low cost；Meanwhile the SnNb of preparation2O6Nanometer sheet has the characteristics that purity is high, good crystallinity,
It can largely synthesize；The SnNb2O6When cathode of the nanometer sheet as lithium ion battery, so that capacity of lithium ion battery is high, cyclicity
It can be good.
The present invention is to be achieved through the following technical solutions:
The invention discloses a kind of SnNb2O6The preparation method of nanometer sheet, comprising the following steps:
1) according to 0.7g:(0.4-1) g:(30-60) mL solid-liquid ratio claim/measure K8Nb6O19、SnCl2·2H2O and ethyl alcohol
Aqueous solution is thoroughly mixed uniformly, mixed solution is made；
2) cooling by mixed solution after 120-200 DEG C of hydro-thermal reaction 2h-12h, through centrifugation, washing, drying, obtain
SnNb2O6Nanometer sheet.
In step 1), the mass percent of dehydrated alcohol is 20%-60% in ethanol water.
In step 1), stir as magnetic agitation.
It is cooling to use cooled to room temperature in step 2).
In step 2), washing is respectively washed for several times using deionized water and dehydrated alcohol.
In step 2), drying temperature is 30-70 DEG C, drying time 1h.
The invention also discloses using SnNb made from the above method2O6Nanometer sheet；And use SnNb2O6Nanometer sheet system
Mass percent is (70-80): (5-10): the SnNb of (15-20) by the method for standby negative electrode of lithium ion battery2O6Nanometer sheet, carboxylic
After sodium carboxymethylcellulose pyce and acetylene black mixed grinding, add water to be configured to mixed slurry, be uniformly coated on copper sheet, obtain lithium from
Sub- battery cathode.
Compared with prior art, the invention has the following beneficial technical effects:
SnNb disclosed by the invention2O6The preparation method of nanometer sheet, using K8Nb6O19、SnCl2·2H2O and ethyl alcohol are water-soluble
Liquid prepares SnNb through cooling, washing, drying by hydro-thermal reaction2O6Nanometer sheet.It is compared to traditional solid phase method, this hair
Bright disclosed preparation method has many advantages, such as easy to operate, at low cost.
Use SnNb made from the preparation method2O6Nanometer sheet purity is high, good crystallinity, repeatability is high, can largely close
At.
SnNb2O6Nanometer sheet has typical layer structure, and this unique crystal structure facilitates the migration of carrier.
Use SnNb2O6Nanometer sheet is as the capacity of lithium ion battery height of working electrode, good cycle.
Detailed description of the invention
Fig. 1 is SnNb prepared by the present invention2O6X-ray diffraction (XRD) map of nanometer sheet；
Fig. 2 is SnNb prepared by the present invention2O6Scanning electron microscope (SEM) photo of nanometer sheet；
Fig. 3 is SnNb prepared by the present invention2O6Transmission electron microscope (TEM) photo of nanometer sheet；
Fig. 4 is SnNb prepared by the present invention2O6The capacity voltage curve of nanometer sheet；
Fig. 5 is SnNb prepared by the present invention2O6The cycle performance figure of nanometer sheet；
Fig. 6 is SnNb prepared by the present invention2O6The high rate performance figure of nanometer sheet.
Specific embodiment
Below with reference to specific embodiment, the present invention is described in further detail, it is described be explanation of the invention and
It is not to limit.
Embodiment 1
SnNb2O6The preparation method of nanometer sheet:
1) title/measurement 0.7g K8Nb6O19, 0.4g SnCl2·2H2The ethyl alcohol that O and 30mL mass fraction is 30% is water-soluble
Liquid is placed in the reaction kettle that liner is polytetrafluoroethylene (PTFE), is thoroughly mixed uniformly using magnetic agitation, mixed solution is made；
2) reaction kettle is put into baking oven, mixed solution is in 120 DEG C of hydro-thermal reaction 2h, and the substance that hydro-thermal reaction is generated is certainly
It is so cooled to room temperature, substance after cooling is centrifuged, vacuum drying is put into using deionized water and dehydrated alcohol washing afterwards for several times
Case, 30 DEG C of dry 1h, obtains SnNb2O6Nanometer sheet.
Using obtained SnNb2O6The method of nanometer sheet production negative electrode of lithium ion battery:
The SnNb that will be obtained2O6Nanometer sheet, sodium carboxymethylcellulose and acetylene black are mixed according to the mass percent of 70:10:20
After closing grinding, adds water to be configured to mixed slurry, be uniformly coated on copper sheet, the cathode as lithium ion battery.
Embodiment 2
SnNb2O6The preparation method of nanometer sheet:
1) title/measurement 0.7g K8Nb6O19, 0.6g SnCl2·2H2The ethyl alcohol that O and 40mL mass fraction is 40% is water-soluble
Liquid is placed in the reaction kettle that liner is polytetrafluoroethylene (PTFE), is thoroughly mixed uniformly using magnetic agitation, mixed solution is made；
2) reaction kettle is put into baking oven, mixed solution is in 160 DEG C of hydro-thermal reaction 8h, and the substance that hydro-thermal reaction is generated is certainly
It is so cooled to room temperature, substance after cooling is centrifuged, vacuum drying is put into using deionized water and dehydrated alcohol washing afterwards for several times
Case, 50 DEG C of dry 1h, obtains SnNb2O6Nanometer sheet.
Using obtained SnNb2O6The method of nanometer sheet production negative electrode of lithium ion battery:
The SnNb that will be obtained2O6Nanometer sheet, sodium carboxymethylcellulose and acetylene black are mixed according to the mass percent of 75:10:15
After closing grinding, adds water to be configured to mixed slurry, be uniformly coated on copper sheet, the cathode as lithium ion battery.
Embodiment 3
SnNb2O6The preparation method of nanometer sheet:
1) title/measurement 0.7g K8Nb6O19, 1g SnCl2·2H2The ethyl alcohol that O and 50mL mass fraction is 50% is water-soluble
Liquid is placed in the reaction kettle that liner is polytetrafluoroethylene (PTFE), is thoroughly mixed uniformly using magnetic agitation, mixed solution is made；
2) reaction kettle is put into baking oven, mixed solution is in 200 DEG C of hydro-thermal reaction 12h, the substance that hydro-thermal reaction is generated
Substance after cooling is centrifuged by cooled to room temperature, and it is dry to be put into vacuum afterwards for several times using deionized water and dehydrated alcohol washing
Dry case, 60 DEG C of dry 1h, obtains SnNb2O6Nanometer sheet.
Using obtained SnNb2O6The method of nanometer sheet production negative electrode of lithium ion battery:
The SnNb that will be obtained2O6Nanometer sheet, sodium carboxymethylcellulose and acetylene black are mixed according to the mass percent of 80:5:15
After closing grinding, adds water to be configured to mixed slurry, be uniformly coated on copper sheet, the cathode as lithium ion battery.
Embodiment 4
SnNb2O6The preparation method of nanometer sheet:
1) title/measurement 0.7g K8Nb6O19, 0.8g SnCl2·2H2The ethyl alcohol that O and 60mL mass fraction is 60% is water-soluble
Liquid is placed in the reaction kettle that liner is polytetrafluoroethylene (PTFE), is thoroughly mixed uniformly using magnetic agitation, mixed solution is made；
2) reaction kettle is put into baking oven, mixed solution is in 180 DEG C of hydro-thermal reaction 6h, and the substance that hydro-thermal reaction is generated is certainly
It is so cooled to room temperature, substance after cooling is centrifuged, vacuum drying is put into using deionized water and dehydrated alcohol washing afterwards for several times
Case, 70 DEG C of dry 1h, obtains SnNb2O6Nanometer sheet.
Using obtained SnNb2O6The method of nanometer sheet production negative electrode of lithium ion battery:
The SnNb that will be obtained2O6Nanometer sheet, sodium carboxymethylcellulose and acetylene black are mixed according to the mass percent of 70:10:20
After closing grinding, adds water to be configured to mixed slurry, be uniformly coated on copper sheet, the cathode as lithium ion battery.
Embodiment 5
SnNb2O6The preparation method of nanometer sheet:
1) title/measurement 0.7g K8Nb6O19, 0.7g SnCl2·2H2The ethyl alcohol that O and 40mL mass fraction is 20% is water-soluble
Liquid is placed in the reaction kettle that liner is polytetrafluoroethylene (PTFE), is thoroughly mixed uniformly using magnetic agitation, mixed solution is made；
2) reaction kettle is put into baking oven, mixed solution is in 140 DEG C of hydro-thermal reaction 10h, the substance that hydro-thermal reaction is generated
Substance after cooling is centrifuged by cooled to room temperature, and it is dry to be put into vacuum afterwards for several times using deionized water and dehydrated alcohol washing
Dry case, 60 DEG C of dry 1h, obtains SnNb2O6Nanometer sheet.
Using obtained SnNb2O6The method of nanometer sheet production negative electrode of lithium ion battery:
The SnNb that will be obtained2O6Nanometer sheet, sodium carboxymethylcellulose and acetylene black are mixed according to the mass percent of 75:5:20
After closing grinding, adds water to be configured to mixed slurry, be uniformly coated on copper sheet, the cathode as lithium ion battery.
Embodiment 6
SnNb2O6The preparation method of nanometer sheet:
1) title/measurement 0.7g K8Nb6O19, 0.5g SnCl2·2H2The ethyl alcohol that O and 30mL mass fraction is 30% is water-soluble
Liquid is placed in the reaction kettle that liner is polytetrafluoroethylene (PTFE), is thoroughly mixed uniformly using magnetic agitation, mixed solution is made；
2) reaction kettle is put into baking oven, mixed solution is in 200 DEG C of hydro-thermal reaction 4h, and the substance that hydro-thermal reaction is generated is certainly
It is so cooled to room temperature, substance after cooling is centrifuged, vacuum drying is put into using deionized water and dehydrated alcohol washing afterwards for several times
Case, 40 DEG C of dry 1h, obtains SnNb2O6Nanometer sheet.
Using obtained SnNb2O6The method of nanometer sheet production negative electrode of lithium ion battery:
The SnNb that will be obtained2O6Nanometer sheet, sodium carboxymethylcellulose and acetylene black are mixed according to the mass percent of 70:10:20
After closing grinding, adds water to be configured to mixed slurry, be uniformly coated on copper sheet, the cathode as lithium ion battery.
Using SnNb produced by the present invention2O6Lithium ion battery of the nanometer sheet as cathode, just extremely lithium metal, electrolyte
It is 1mol/L LiPF6EC+DEC+DMC (EC/DEC/DMC=1/1/1, v/v/v) solution.All assemblings are being full of argon gas
Glove box in carry out.
It will be seen from figure 1 that the object of nanometer sheet prepared by the present invention is mutually SnNb2O6, compared with standard card, feature is spread out
Peak is penetrated to fit like a glove.It can be seen that prepared SnNb from Fig. 2, Fig. 32O6Nanometer sheet surface is smooth, intersects between nanometer sheet and combines
Form a large amount of holes；It can be seen that SnNb from Fig. 4, Fig. 5 and Fig. 62O6Electrode is 0.1Ag in current density-1Under the conditions of recycle 50
When circle, specific capacity is 519mAh g-1.It is 0.2A g in current density-1、0.5A g-1、1.0A g-1、2.0A g-1Under the conditions of point
Not Xun Huan 10 circle, SnNb2O6The specific capacity of electrode is respectively 486mAh g-1、425mAh g-1、358mAh g-1、304mAh g-1,
Show it with good cycle performance and high rate performance.
Claims (9)
1. a kind of SnNb2O6The preparation method of nanometer sheet, which comprises the following steps:
1) according to 0.7g:(0.4-1) g:(30-60) mL solid-liquid ratio claim/measure K8Nb6O19、SnCl2·2H2O and ethyl alcohol are water-soluble
Liquid is thoroughly mixed uniformly, mixed solution is made；
2) cooling by mixed solution after 120-200 DEG C of hydro-thermal reaction 2h-12h, through centrifugation, washing, drying, obtain SnNb2O6
Nanometer sheet.
2. SnNb according to claim 12O6The preparation method of nanometer sheet, which is characterized in that in step 1), ethyl alcohol is water-soluble
The mass percent of dehydrated alcohol is 20%-60% in liquid.
3. SnNb according to claim 12O6The preparation method of nanometer sheet, which is characterized in that in step 1), stir as magnetic
Power stirring.
4. SnNb according to claim 12O6The preparation method of nanometer sheet, which is characterized in that cooling to use in step 2)
Cooled to room temperature.
5. SnNb according to claim 12O6The preparation method of nanometer sheet, which is characterized in that in step 2), washing is used
Deionized water and dehydrated alcohol respectively wash for several times.
6. SnNb according to claim 12O6The preparation method of nanometer sheet, which is characterized in that in step 2), drying temperature
30-70 DEG C of drying time is 1h.
7. using SnNb made from any one of claim 1-6 preparation method2O6Nanometer sheet.
8. SnNb as claimed in claim 72O6Nanometer sheet is preparing the application in lithium battery.
9. using SnNb as claimed in claim 72O6The method that nanometer sheet prepares negative electrode of lithium ion battery, it is characterised in that: by matter
Measuring percentage is (70-80): (5-10): the SnNb of (15-20)2O6Nanometer sheet, sodium carboxymethylcellulose and acetylene black mixed grinding
Afterwards, add water to be configured to mixed slurry, be uniformly coated on copper sheet, obtain negative electrode of lithium ion battery.
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| CN201811004710.6A CN109133172A (en) | 2018-08-30 | 2018-08-30 | A kind of niobic acid tin nanometer sheet and preparation method thereof and preparing the application in lithium battery |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113675388A (en) * | 2021-07-20 | 2021-11-19 | 苏州科技大学 | Nitrogen-doped carbon-coated tin niobate nano material and preparation method and application thereof |
| CN113666420A (en) * | 2021-08-28 | 2021-11-19 | 济南大学 | Bimetal niobium oxide and carbon composite material thereof, preparation method and application |
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| CN106944035A (en) * | 2017-02-27 | 2017-07-14 | 陕西科技大学 | A kind of oxygen auto-dope stratiform niobium oxide powder and its preparation method and application |
| CN107601564A (en) * | 2017-09-04 | 2018-01-19 | 北京工业大学 | A kind of method of alcoholic solvent hot preparation niobic acid tin nanosphere |
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2018
- 2018-08-30 CN CN201811004710.6A patent/CN109133172A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106944035A (en) * | 2017-02-27 | 2017-07-14 | 陕西科技大学 | A kind of oxygen auto-dope stratiform niobium oxide powder and its preparation method and application |
| CN107601564A (en) * | 2017-09-04 | 2018-01-19 | 北京工业大学 | A kind of method of alcoholic solvent hot preparation niobic acid tin nanosphere |
Non-Patent Citations (4)
| Title |
|---|
| CHAO ZHOU等: "Facile synthesis of ultrathin SnNb2O6 nanosheets towards improved visible-light photocatalytic H2-production activity", 《CHEM. COMMUN.》 * |
| CHAO ZHOU等: "Two‐step hydrothermal synthesis of Sn2Nb2O7 nanocrystals with enhanced visible‐light‐driven H2 evolution activity", 《CHINESE JOURNAL OF CATALYSIS》 * |
| PENGBO ZHAI等: "Smart hybridization of Sn2Nb2O7/SnO2@3D carbon nanocomposites with enhanced sodium storage performance through self-buffering effects", 《JOURNAL OF MATERIALS CHEMISTRY A》 * |
| 李开翻: "层状SnNb2O6的制备及其光电化学性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113675388A (en) * | 2021-07-20 | 2021-11-19 | 苏州科技大学 | Nitrogen-doped carbon-coated tin niobate nano material and preparation method and application thereof |
| CN113675388B (en) * | 2021-07-20 | 2022-06-28 | 苏州科技大学 | Nitrogen-doped carbon-coated tin niobate nano material and preparation method and application thereof |
| CN113666420A (en) * | 2021-08-28 | 2021-11-19 | 济南大学 | Bimetal niobium oxide and carbon composite material thereof, preparation method and application |
| CN113666420B (en) * | 2021-08-28 | 2022-07-08 | 济南大学 | Bimetal niobium oxide and carbon composite material thereof, preparation method and application |
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Application publication date: 20190104 |
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| RJ01 | Rejection of invention patent application after publication |