CN107293411A - A kind of quick method for preparing tin ash two dimension carbonization titanium composite material - Google Patents
A kind of quick method for preparing tin ash two dimension carbonization titanium composite material Download PDFInfo
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- CN107293411A CN107293411A CN201710425742.2A CN201710425742A CN107293411A CN 107293411 A CN107293411 A CN 107293411A CN 201710425742 A CN201710425742 A CN 201710425742A CN 107293411 A CN107293411 A CN 107293411A
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- tin
- composite material
- titanium composite
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- dimension
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The present invention relates to a kind of quick method for preparing tin ash two dimension carbonization titanium composite material, belong to field of material preparation.Two-dimentional titanium carbide is added in the compound water solution of tin by the present invention to be well mixed, then using microwave fast heating mixed solution, so as to prepare tin ash two dimension carbonization titanium composite material.The preparation method is easy, it is with low cost, target product can be quickly prepared in normal temperature environment, and the method heated using microwave is easy to industrial mass production, obtained tin ash two dimension carbonization titanium composite material can be used for ultracapacitor, the electrode material of lithium ion battery.
Description
Technical field
The present invention relates to a kind of quick method for preparing tin ash-two dimension carbonization titanium composite material, belong to material preparation
Field.
Background technology
Research finds, two-dimentional transition metal carbide and/or nitride (MXene) are as a kind of electric conductivity is good and table
The regulatable two-dimensional layer material of face functional group, have in energy storage field great application prospect (Naguib, M., et al.,
Advanced Materials,2014.26(7):992-1005).Wherein two-dimentional titanium carbide (Ti3C2) it is a kind of typical MXene
Material, available for the preparation of lithium ion battery and the electrode material of ultracapacitor, but Ti3C2Interlayer easily collapse and heap
Pile together, influences it as the performance of electrode material.The trend of current main flow is by Ti3C2It is compound with other materials, to prevent
Ti3C2Stacking so that reduce ion-transfer resistance and increase ion adsorption site.In Ti such as Rakhi3C2Upper original
Position growth ε-MnO2It is nanocrystalline, weight ratio capacity (Rakhi, R.B., the et al., ACS of composite can be dramatically increased
Applied Materials&Interfaces,2016.8(29):18806-18814)。
Tin ash (SnO2) due to its abundant resource, relatively low price and good capacitance characteristic, it is a kind of potential
Electrode material.But its electric conductivity is poor, and serious Volume Changes are there are in charge and discharge process, have impact on
SnO2Further apply.If by SnO2Growth in situ is in Ti3C2On synusia, SnO can be effectively prevented2Reunion and extension
Ti3C2The synusia spacing of matrix, is conducive to the diffusion and absorption of electrolyte ion, so as to improve Ti3C2Energy-storage property.
It is less efficient but the method that tradition prepares tin ash-two dimension carbonization titanium composite material is comparatively laborious, therefore,
It is to promote an urgent demand of tin ash-two dimension titanium carbide to seek a kind of efficient, cheap method.
The content of the invention
Technical problem：It is carbonized titanium composite material it is an object of the invention to provide a kind of quick tin ash-two dimension for preparing
Method, this method is simple to operate, quick, with low cost, can be mass-produced.
Technical scheme：, should the invention provides a kind of quick method for preparing tin ash-two dimension carbonization titanium composite material
Method comprises the following steps：
1) it is well mixed in the compound solution that two-dimentional titanium carbide is added to tin, obtains mixed solution；
2) by step 1) heating of mixed solution microwave is obtained, drying is then centrifuged for, described tin ash-Two-dimensional Carbon is obtained
Change titanium composite material.
Wherein：
The compound solution of described tin is that stannous chloride solution, tin chloride solution, nitric acid solution of tin, nitric acid stannous are molten
Tin in one or more mixed solutions in liquid, stannous sulfate solution or stannous acetate solution, the compound solution of the tin
Concentration range be 0.1~10mol/L.
The mass ratio of the compound of the two-dimentional titanium carbide and tin is 0.1~100.
It is described it is well mixed refer to by electromagnetic agitation, be stirring under conditions of 20~100 hertz in stirring frequency
0.5~24h.
The power of described microwave heating is 700~1800 watts, and the heat time is 5~300s.
The centrifugation refers to centrifuge 1~20min in the case where rotating speed is 1000~10000rpm centrifugation rate, abandoned afterwards
Clear liquid, distilled water is added into sediment, is centrifuged again, repeated centrifugation more than 3 times；Described drying refers to the production after centrifugation
Thing is placed in baking oven or drying box, under conditions of temperature is 25~70 DEG C, is dried 5~40 hours.
In order to improve the yield of tin ash-two dimension carbonization titanium composite material, to step 1) obtain mixed solution microwave
During heating operation, to mixed solution, microwave is heated repeatedly, and follow-up centrifugal drying operation is carried out afterwards.
Beneficial effect：Compared with the conventional method, the invention has the advantages that：
1. equipment investment is few, the simple to operate, cycle is short, less energy consumption, with low cost, easily realizes large-scale production, preparation process
It is safe and reliable pollution-free；
2. the method heated using microwave prepares tin ash-two dimension carbonization titanium composite material, the time only needs 5~300 seconds,
The conventional method that compares (in hours), the production time significantly shortens, and production efficiency is significantly improved.
Brief description of the drawings
Fig. 1 schemes for the tin ash-two dimension carbonization titanium composite material SEM prepared in the embodiment of the present invention 1；
Fig. 2 is carbonized titanium composite material as super capacitor electrode for the tin ash-two dimension prepared in the embodiment of the present invention 1
The constant current charge-discharge curve of pole.
Embodiment
In order to reach object above, the method for tin ash-two dimension carbonization titanium composite material of the invention includes following base
This step：
1. mixing：The compound solution of two-dimentional titanium carbide and tin is stirred；
2. microwave is heated：The beaker for being contained with mixed solution is placed in microwave device and quickly heated, so as to prepare rapidly
Tin ash-two dimension carbonization titanium composite material.
It should be noted that can be to mixed solution after being cooled down by the heating of first time microwave, heating for multiple times, to improve two
The yield of tin oxide-two dimension carbonization titanium composite material.
Embodiment 1：
1. mixing：The two-dimentional titanium carbide of the weight such as addition in the polytetrafluoroethylene beaker for being contained with 100mL distilled water
(200mg) and stannous chloride dihydrate (2000mg), electromagnetic agitation 0.5h, obtains mixed solution, wherein stirring frequency is 20 afterwards
Hertz；
2. microwave is heated：The polytetrafluoroethylene beaker for holding mixed solution in step 1 is placed in microwave device, with
Quick heating 300 seconds of 700 watts of power, centrifuge 20min to reaction solution under conditions of rotating speed is 1000rpm afterwards, will be from
Heart product is placed in drying box, under conditions of temperature is 25 DEG C, dries 40h, you can obtain target product.
Embodiment 2：
1. mixing：The two-dimentional titanium carbide of the weight such as addition in the polytetrafluoroethylene beaker for being contained with 100mL distilled water
(200mg) and stannous chloride dihydrate (10mg), electromagnetic agitation 24h, obtains mixed solution, wherein stirring frequency is 50 hertz afterwards
Hereby；
2. microwave is heated：The polytetrafluoroethylene beaker for holding mixed solution in step 1 is placed in microwave device, with
1800 watts of power is quickly heated 5 seconds, is centrifuged 10min under conditions of rotating speed is 4000rpm to reaction solution afterwards, will be centrifuged
Product is placed in baking oven, under conditions of temperature is 50 DEG C, dries 20h, you can obtain target product.
Embodiment 3：
1. mixing：Two-dimentional titanium carbide (200mg) and two are added in the polytetrafluoroethylene beaker for being contained with 100mL distilled water
Water stannous chloride (200mg), electromagnetic agitation 12h, obtains mixed solution, wherein stirring frequency is 100 hertz afterwards；；
2. microwave is heated：The polytetrafluoroethylene beaker for holding mixed solution in step 1 is placed in microwave device, with
900 watts of power is quickly heated 40 seconds, is centrifuged 1min under conditions of rotating speed is 10000rpm to reaction solution afterwards, will be centrifuged
Product is placed in drying box, under conditions of temperature is 70 DEG C, dries 5h, you can obtain target product.
Embodiment 4：
1. mixing：The two-dimentional titanium carbide of the weight such as addition in the polytetrafluoroethylene beaker for being contained with 100mL distilled water
(2000mg) and stannic chloride pentahydrate (20mg), electromagnetic agitation 24h, obtains mixed solution, wherein stirring frequency is 70 hertz afterwards
Hereby；
2. microwave is heated：The polytetrafluoroethylene beaker for holding mixed solution in step 1 is placed in microwave device, with
Quick heating 120 seconds of 1500 watts of power, centrifuge 15min to reaction solution under conditions of rotating speed is 8000rpm afterwards, will be from
Heart product is placed in drying box, under conditions of temperature is 60 DEG C, dries 30h, you can obtain target product.
In addition to the implementation, the present invention can also have other embodiment, all use equivalent substitution or equivalent transformation shape
Into technical scheme, belong to the protection domain of application claims.
Claims (6)
1. a kind of quick method for preparing tin ash-two dimension carbonization titanium composite material, it is characterised in that：This method includes as follows
Step：
1) it is well mixed in the compound solution that two-dimentional titanium carbide is added to tin, obtains mixed solution；
2) by step 1) heating of mixed solution microwave is obtained, it is then centrifuged for drying, you can obtain described tin ash-Two-dimensional Carbon
Change titanium composite material.
The preparation method of titanium composite material 2. tin ash according to claim 1-two dimension is carbonized, it is characterised in that：Institute
The compound solution for the tin stated is stannous chloride solution, tin chloride solution, nitric acid solution of tin, nitric acid stannous solution, stannous sulfate
The concentration range of tin is in one or more mixed solutions in solution or stannous acetate solution, the compound solution of the tin
0.1~10mol/L.
The preparation method of titanium composite material 3. tin ash according to claim 1-two dimension is carbonized, it is characterised in that：Institute
The mass ratio for stating the compound of two-dimentional titanium carbide and tin is 0.1~100.
The preparation method of titanium composite material 4. tin ash according to claim 1-two dimension is carbonized, it is characterised in that：Institute
State it is well mixed refer to by electromagnetic agitation, stirring frequency be 20~100 hertz under conditions of, stir 0.5~24h.
The preparation method of titanium composite material 5. tin ash according to claim 1-two dimension is carbonized, it is characterised in that：Institute
The power for the microwave heating stated is 700~1800 watts, and the heat time is 5~300s.
The preparation method of titanium composite material 6. tin ash according to claim 1-two dimension is carbonized, it is characterised in that：Institute
State centrifugation to refer to centrifuge 1~20min in the case where rotating speed is 1000~10000rpm centrifugation rate, supernatant, Xiang Chen are abandoned afterwards
Distilled water is added in starch, is centrifuged again, repeated centrifugation more than 3 times；Described drying refers to the product after centrifugation being placed in baking
In case or drying box, under conditions of temperature is 25~70 DEG C, dry 5~40 hours.
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| CN201710425742.2A CN107293411A (en) | 2017-06-08 | 2017-06-08 | A kind of quick method for preparing tin ash two dimension carbonization titanium composite material |
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| CN201710425742.2A CN107293411A (en) | 2017-06-08 | 2017-06-08 | A kind of quick method for preparing tin ash two dimension carbonization titanium composite material |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1796287A (en) * | 2004-12-30 | 2006-07-05 | 广东工业大学 | Method for preparing Nano granules of stannic oxide |
| CN104143631A (en) * | 2014-05-12 | 2014-11-12 | 上海大学 | Method for preparing graphene aerogel loaded tin dioxide composite material |
| CN105720246A (en) * | 2015-12-25 | 2016-06-29 | 陕西科技大学 | Granular tin dioxide/two-dimensional nanometer titanium carbide composite material and application thereof |
-
2017
- 2017-06-08 CN CN201710425742.2A patent/CN107293411A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1796287A (en) * | 2004-12-30 | 2006-07-05 | 广东工业大学 | Method for preparing Nano granules of stannic oxide |
| CN104143631A (en) * | 2014-05-12 | 2014-11-12 | 上海大学 | Method for preparing graphene aerogel loaded tin dioxide composite material |
| CN105720246A (en) * | 2015-12-25 | 2016-06-29 | 陕西科技大学 | Granular tin dioxide/two-dimensional nanometer titanium carbide composite material and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 韩凤兰，孙强，李良学，任江涛: ""微波法制取二氧化锡粉体材料"", 《石油化工应用》 * |
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