CN101704548A - Method for preparing stannous oxide nano material in cross sheet structure by thermal decomposition - Google Patents
Method for preparing stannous oxide nano material in cross sheet structure by thermal decomposition Download PDFInfo
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- CN101704548A CN101704548A CN200910153717A CN200910153717A CN101704548A CN 101704548 A CN101704548 A CN 101704548A CN 200910153717 A CN200910153717 A CN 200910153717A CN 200910153717 A CN200910153717 A CN 200910153717A CN 101704548 A CN101704548 A CN 101704548A
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Abstract
The invention discloses a method for preparing a stannous oxide nano material in cross sheet structure by thermal decomposition, comprising the following steps: dissolving tetraphenyltin in dissolvent to prepare 5.5mmol/L to 110mmol/L of tetraphenyltin solution; placing the obtained solution in a container and then heating to 260-310 DEG C; keeping the temperature and refluxing for 0.5h-4h; centrifuging, washing and drying the obtained solid product to obtain black powder, namely the stannous oxide nano material in cross sheet structure. The method can reduce reaction cost and improve production efficiency of the stannous oxide nano material, and the prepared nano material has a special cross sheet structure and good repeatability.
Description
Technical field
The present invention relates to field of nano material preparation, particularly relate to a kind of method of preparing stannous oxide nano material in cross sheet structure by thermal decomposition.
Background technology
Nano material and nanostructure be the most dynamic in the current novel material research field, the future economy and social development are had the very research object of material impact, also be the most active in the nanosecond science and technology, the important component part of approaching application.
Tin protoxide is very important a kind of in the metal oxide materials, it is a kind of semiconductor material, in organic synthesis, plating, glass industry, solar cell and lithium-ion secondary cell,, thereby become the emphasis of people research by extensive studies and application.Hydrothermal method is passed through in existing at present research, liquid phase method, and microwave method, ultrasonic method, thermal evaporation, electron-beam vapor deposition methods etc. have prepared the tin protoxide nanoparticle, nano belt, nanometer flower, nanometer sheet, film, whisker or the like.Above method all can prepare the tin protoxide material with nanostructure, but reaction conditions relative complex all, long reaction time, output is also relatively low.Advantage is considered to one of following method for preparing the potentialization of some practicability nano material to thermal decomposition method because the product cost of preparation is low, equipment is simple, controllability is good etc.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing stannous oxide nano material in cross sheet structure by thermal decomposition, this method has that reaction conditions is simple, the reaction times is short, output is big, product purity is high and advantage such as product property is superior.
The step of the technical solution used in the present invention is as follows:
(1) tin tetraphenyl is dissolved in the solvent, prepares the tin tetraphenyl solution of 5.5mmol/L～110mmol/L;
(2) solution that obtains in (1) step is inserted vessel in heating to 260 ℃～310 ℃, insulation backflow 0.5h～4h, the solid product of gained obtains black powder after centrifugal, washing, drying, be stannous oxide nano material in cross sheet structure.
At the described solvent of (1) step is octadecylene or trioctylamine.
The beneficial effect that the present invention has is:
1) this preparation method is simple, and cost is low, and condition is so not harsh relatively;
2) product purity height is not introduced other impurity, productive rate＞95%;
3) have special cross sheet structure, have good repeatability.
Description of drawings
Fig. 1 is the stereoscan photograph of the stannous oxide nano material in cross sheet structure of embodiment 1 preparation.
Fig. 2 is that the XRD of the stannous oxide nano material in cross sheet structure of embodiment 1 preparation characterizes.
Embodiment
Embodiment 1:
Carry out according to preparation process. the 0.1g tin tetraphenyl is added there-necked flask, add the 20ml octadecylene, magnetic agitation 5 minutes, obtain translucent white turbid solution. the there-necked flask of reaction soln will be housed, place in the controlled heating jacket of temperature intelligent and continue to heat, reaction conditions is: 310 ℃, 2h. the solid normal temperature vacuum-drying powdered that obtains after centrifugal repeatedly 5 times of reaction back solution centrifugal 5min. under the 3000r/min centrifugation rate. the sem test sample then is that sample is sticked on the aluminium base sample table, Fig. 1 has provided the stereoscan photograph of the stannous oxide nano material in cross sheet structure that obtains according to embodiment 1. can obviously find out stannous oxide nano material in cross sheet structure whole pattern roughly from Fig. 1. and Fig. 2 characterizes for the stannous oxide nano material in cross sheet structure XRD that obtains according to embodiment 1, as can be seen from the figure stannous oxide nano material in cross sheet structure perfect crystalline and free from foreign meter.
Embodiment 2:
Carry out according to preparation process.The 0.05g tin tetraphenyl is added there-necked flask, add the 20ml octadecylene, magnetic agitation 5 minutes obtains translucent white turbid solution.To the there-necked flask of reaction soln be housed, place in the controlled heating jacket of temperature intelligent to continue to heat, reaction conditions is: 310 ℃, and 2h.Reaction back solution centrifugal 5min under the 3000r/min centrifugation rate.The solid normal temperature vacuum-drying powdered that obtains after centrifugal repeatedly 5 times.Product is a stannous oxide nano material in cross sheet structure, and pattern and embodiment 1 are similar.
Embodiment 3:
Carry out according to preparation process.The 1g tin tetraphenyl is added there-necked flask, add the 20ml octadecylene, magnetic agitation 5 minutes obtains translucent white turbid solution.To the there-necked flask of reaction soln be housed, place in the controlled heating jacket of temperature intelligent to continue to heat, reaction conditions is: 310 ℃, and 2h.Reaction back solution centrifugal 5min under the 3000r/min centrifugation rate.The solid normal temperature vacuum-drying powdered that obtains after centrifugal repeatedly 5 times.Product is a stannous oxide nano material in cross sheet structure, and pattern and embodiment 1 are similar.
Embodiment 4:
Carry out according to preparation process.The 0.1g tin tetraphenyl is added there-necked flask, add the 20ml trioctylamine, magnetic agitation 5 minutes obtains translucent white turbid solution.To the there-necked flask of reaction soln be housed, place in the controlled heating jacket of temperature intelligent to continue to heat, reaction conditions is: 310 ℃, and 2h.Reaction back solution centrifugal 5min under the 3000r/min centrifugation rate.The solid normal temperature vacuum-drying powdered that obtains after centrifugal repeatedly 5 times.Product is a stannous oxide nano material in cross sheet structure, and pattern and embodiment 1 are similar.
Embodiment 5:
Carry out according to preparation process.The 0.1g tin tetraphenyl is added there-necked flask, add the 20ml octadecylene, magnetic agitation 5 minutes obtains translucent white turbid solution.To the there-necked flask of reaction soln be housed, place in the controlled heating jacket of temperature intelligent to continue to heat, reaction conditions is: 260 ℃, and 2h.Reaction back solution centrifugal 5min under the 3000r/min centrifugation rate.The solid normal temperature vacuum-drying powdered that obtains after centrifugal repeatedly 5 times.Product is a stannous oxide nano material in cross sheet structure, and pattern and embodiment 1 are similar.
Embodiment 6:
Carry out according to preparation process.The 0.1g tin tetraphenyl is added there-necked flask, add the 20ml octadecylene, magnetic agitation 5 minutes obtains translucent white turbid solution.To the there-necked flask of reaction soln be housed, place in the controlled heating jacket of temperature intelligent to continue to heat, reaction conditions is: 280 ℃, and 2h.Reaction back solution centrifugal 5min under the 3000r/min centrifugation rate.The solid normal temperature vacuum-drying powdered that obtains after centrifugal repeatedly 5 times.Product is a stannous oxide nano material in cross sheet structure, and pattern and embodiment 1 are similar.
Embodiment 7:
Carry out according to preparation process. the 0.1g tin tetraphenyl is added there-necked flask, add the 20ml octadecylene, magnetic agitation 5 minutes, obtain translucent white turbid solution. the there-necked flask of reaction soln will be housed, place in the controlled heating jacket of temperature intelligent and continue to heat, reaction conditions is: 310 ℃, 0.5h. the solid normal temperature vacuum-drying powdered that obtains after centrifugal repeatedly 5 times of reaction back solution centrifugal 5min. under the 3000r/min centrifugation rate. product is a stannous oxide nano material in cross sheet structure, and pattern and embodiment 1 are similar.
Embodiment 8:
Carry out according to preparation process.The 0.1g tin tetraphenyl is added there-necked flask, add the 20ml octadecylene, magnetic agitation 5 minutes obtains translucent white turbid solution.To the there-necked flask of reaction soln be housed, place in the controlled heating jacket of temperature intelligent to continue to heat, reaction conditions is: 310 ℃, and 4h.Reaction back solution centrifugal 5min under the 3000r/min centrifugation rate.The solid normal temperature vacuum-drying powdered that obtains after centrifugal repeatedly 5 times.Product is a stannous oxide nano material in cross sheet structure, and pattern and embodiment 1 are similar.
Claims (2)
1. the method for a preparing stannous oxide nano material in cross sheet structure by thermal decomposition is characterized in that the step of this method is as follows:
(1) tin tetraphenyl is dissolved in the solvent, prepares the tin tetraphenyl solution of 5.5mmol/L～110mmol/L;
(2) solution that obtains in (1) step is inserted vessel in heating to 260 ℃～310 ℃, insulation backflow 0.5h～4h, the solid product of gained obtains black powder after centrifugal, washing, drying, be stannous oxide nano material in cross sheet structure.
2. the method for a kind of preparing stannous oxide nano material in cross sheet structure by thermal decomposition according to claim 1, it is characterized in that: at the described solvent of (1) step is octadecylene or trioctylamine.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109935824A (en) * | 2017-12-15 | 2019-06-25 | 东莞市凯金新能源科技股份有限公司 | A kind of expanded graphite negative electrode material and preparation method thereof loading cross acicular tin oxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109935824A (en) * | 2017-12-15 | 2019-06-25 | 东莞市凯金新能源科技股份有限公司 | A kind of expanded graphite negative electrode material and preparation method thereof loading cross acicular tin oxide |
| CN109935824B (en) * | 2017-12-15 | 2021-05-11 | 广东凯金新能源科技股份有限公司 | Expanded graphite cathode material loaded with cross needle-shaped tin oxide and preparation method thereof |
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Open date: 20100512 |