CN105293571B - A kind of method that utilization metallic tin directly prepares tin oxide nano particles - Google Patents
A kind of method that utilization metallic tin directly prepares tin oxide nano particles Download PDFInfo
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- CN105293571B CN105293571B CN201510860093.XA CN201510860093A CN105293571B CN 105293571 B CN105293571 B CN 105293571B CN 201510860093 A CN201510860093 A CN 201510860093A CN 105293571 B CN105293571 B CN 105293571B
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- nano particles
- tin oxide
- oxide nano
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- iodine
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Abstract
The invention belongs to the preparation field of nano material, and in particular to a kind of method that utilization metallic tin directly prepares tin oxide nano particles.The method is specially during metallic tin is placed in iodine/ethanol and sodium carbonate mixture, and Jing high-temperature water/solvent thermal reaction obtains nano tin dioxide material.The present invention is based on Kirkendall effects, by the inequality diffusion of different material between two-phase interface, so as to form the stannic oxide nanometer grain with nano-grade size.By means of the invention it is possible to directly utilize simple substance stannum to be raw material, tin oxide nano particles are prepared under the conditions of neutral gentle pH is close to, obtain product purity high, organic formwork agent is not used, energy consumption and pollution that high-temperature roasting causes can be avoided, and nanoparticle agglomeration at high temperature can be avoided.
Description
Technical field
The invention belongs to the preparation field of nano material, and in particular to one kind directly prepares titanium dioxide sijna using metallic tin
The method of rice grain.
Background technology
Tin ash (SnO2) it is a kind of important semiconductor material with wide forbidden band.In recent years, the SnO with nanostructured2Material
Expect due to unique optical property, electric property, chemical stability etc., thus catalysis, gas sensitive, senser element,
The aspects such as photoelectric device show important using value.SnO2The application of nano structural material is ground with the innovation of preparation method
Study carefully and have very important significance.
The SnO of high dispersive2Nano-particle has that particle size is little, specific surface area is big, surface energy is high, surface atom institute accounting
The features such as example is big, therefore the SnO of high dispersive2Nano-particle often has higher catalysis activity and vapor sensitivity.
At present, the SnO for proposing both at home and abroad2The preparation method of nano-particle mainly have sol-gel process, chemical precipitation method,
Hydrothermal synthesis method and solid-phase synthesis etc..The particle size that wherein prepared by hydrothermal synthesis method is uniform, and degree of crystallinity is high, pattern rule.
Nano SnO2Synthesis generally with pink salt as raw material, carry out under strongly alkaline conditions, organic formwork agent must also be used sometimes.It is this kind of
Method there are problems that polluting environment, high cost, waste of resource and last handling process.Therefore, one kind is developed gentle
Under pH value, organic formwork agent synthesis SnO is not used2The preparation method of nano-particle has important realistic meaning.
The content of the invention
The present invention is intended to provide a kind of method that utilization metallic tin directly prepares tin oxide nano particles, the method operation
Simply, without the need for strong alkaline condition, carry out under gentle pH value system, organic formwork agent is not used therefore without the need for high-temperature roasting, institute
Obtained SnO2Nanoparticle size is less, by the nanoparticle of a diameter of 10～50nm with monodispersed form or to a certain degree
Aggregate form exist, and can be adjusted according to experiment condition.
The present invention is achieved through the following technical solutions：
A kind of method that utilization metallic tin directly prepares tin oxide nano particles, specifically includes following steps：
(1) a certain amount of elemental iodine is dissolved in dehydrated alcohol, weigh a certain amount of natrium carbonicum calcinatum be dissolved in from
In sub- water, above-mentioned iodine/ethanol solution is mixed with aqueous sodium carbonate, add the metal simple-substance glass putty of amount of calculation, make raw material rub
You are than being Sn: I2∶Na2CO3∶H2O∶C2H5OH=1: 0.5～3.0: 0.05～2.0: 20～200: 10～100, after persistently stirring,
Obtain rufous mixed liquor；
(2) above-mentioned mixed liquor is transferred quickly in stainless steel cauldron, glass putty is all transferred to reactor,
React 1～3 day under the conditions of 180～220 DEG C, naturally cool to room temperature, the solid being centrifugally separating to obtain；
(3) solid that centrifugation is obtained is sequentially passed through into dehydrated alcohol, deionized water wash, is dried, obtained with different points
The tin oxide nano particles of divergence.
Compared with prior art, the present invention has following beneficial technique effect：
The present invention with metallic tin simple substance as raw material, in the case where neutral gentle pH value condition is close to, the I in reaction system2With
Na2CO3In the presence of, tin oxide nano particles are prepared for using hydro-thermal method, purity is high, does not use organic formwork agent, therefore keeps away
The particle aggregation phenomenon that high-temperature roasting may cause is exempted from.Tin oxide nano particles are prepared as raw material with solid-state simple substance stannum, is
Based on Kirkendall effects, (between two-phase interface, different material migration rate is different, i.e. inequality diffusion, can cause cavernous structure
Generation) solid phase transformation route, be that tin dioxide material preparation method is benefited our pursuits.
Description of the drawings
Fig. 1：The X-ray diffractogram of tin ash prepared by the embodiment of the present invention 1.
Fig. 2：The transmission electron microscope picture of tin ash prepared by the embodiment of the present invention 1.
Specific embodiment
The specific embodiment of the present invention is the following is, is that the present invention is further described.But specific embodiment does not limit this
Invention claim.
The raw material arrived used in specific embodiment is as follows：
Sn powder：Tianjin Kermel Chemical Reagent Co., Ltd.；
Iodine：Tianjin Bei Lian fine chemicals development corporation, Ltd.；
Natrium carbonicum calcinatum：Tianjin Kermel Chemical Reagent Co., Ltd..
Embodiment 1：
1.0 grams of elemental iodines are dissolved in 12.5 milliliters of dehydrated alcohol, 0.2 gram of natrium carbonicum calcinatum are weighed in addition and is dissolved in 6.0
In ml deionized water；Above-mentioned iodine/ethanol solution is mixed with aqueous sodium carbonate, 0.4 gram of metal simple-substance glass putty is added, is continued
After stirring, rufous mixed liquor is obtained；Above-mentioned mixed liquor is transferred quickly in stainless steel cauldron, glass putty is all transferred to
Reactor, under the conditions of 280 DEG C react 3 days, naturally cool to room temperature, the solid being centrifugally separating to obtain, successively Jing ethanol, go from
Sub- water washing, is dried, and obtains uniform particle sizes, well dispersed tin oxide nano particles.
Embodiment 2：
2.0 grams of elemental iodines are dissolved in 8.0 milliliters of dehydrated alcohol, 0.8 gram of natrium carbonicum calcinatum are weighed in addition and is dissolved in 6.0 millis
Rise in deionized water；Above-mentioned iodine/ethanol solution is mixed with aqueous sodium carbonate, 0.6 gram of metal simple-substance glass putty is added, is persistently stirred
After mixing, rufous mixed liquor is obtained；Above-mentioned mixed liquor is transferred quickly in stainless steel cauldron, glass putty is all transferred to anti-
Kettle is answered, reaction 1 day, naturally cools to room temperature under the conditions of 220 DEG C, the solid being centrifugally separating to obtain, successively Jing ethanol, deionization
Water washing, is dried, and obtains tin oxide nano particles.
Embodiment 3：
0.65 gram of elemental iodine is dissolved in 5.5 milliliters of dehydrated alcohol, 0.27 gram of natrium carbonicum calcinatum is weighed in addition and is dissolved in 5.5
In ml deionized water；Above-mentioned iodine/ethanol solution is mixed with aqueous sodium carbonate, 0.2 gram of metal simple-substance glass putty is added, is continued
After stirring, rufous mixed liquor is obtained；Above-mentioned mixed liquor is transferred quickly in stainless steel cauldron, glass putty is all transferred to
Reactor, under the conditions of 200 DEG C react 2 days, naturally cool to room temperature, the solid being centrifugally separating to obtain, successively Jing ethanol, go from
Sub- water washing, is dried, and obtains the good tin oxide nano particles of crystallinity.
The above, is only several case study on implementation of the present invention, any pro forma restriction is not done to the present invention, any
Those skilled in the art, in the range of without departing from technical solution of the present invention, when structure and skill using the disclosure above
Art content is made a little change or is modified to the equivalence enforcement case of equivalent variations.But it is every without departing from technical solution of the present invention
Content, according to any simple modification made to above case study on implementation of technical spirit of the present invention, equivalent variations and modification,
Still belong in the range of technical solution of the present invention.
Claims (6)
1. a kind of method that utilization metallic tin directly prepares tin oxide nano particles, it is characterised in that the method is specifically included
The following steps：
(1) a certain amount of elemental iodine is dissolved in dehydrated alcohol, weighs a certain amount of natrium carbonicum calcinatum and be dissolved in deionized water
In, above-mentioned iodine/ethanol solution is mixed with aqueous sodium carbonate, the metal simple-substance glass putty of amount of calculation is added, is made material molar ratio
For Sn: I2∶Na2CO3=1: 0.5～3.0: 0.05～2.0, after persistently stirring, obtain rufous mixed liquor；
(2) above-mentioned mixed liquor is transferred quickly in stainless steel cauldron, glass putty is all transferred to reactor, 180～
React 1～3 day under the conditions of 220 DEG C, naturally cool to room temperature, the solid being centrifugally separating to obtain, washing are dried, and obtain with not
With the tin oxide nano particles of dispersion.
2. method according to claim 1, it is characterised in that the lasting stirring described in step (1) is by mixed solution magnetic
Power stirs 10～120min.
3. method according to claim 1, it is characterised in that the iodine/ethanol solution described in step (1), its mol ratio are I2
∶C2H5OH=1: 10～80.
4. method according to claim 1, it is characterised in that the aqueous sodium carbonate concentration described in step (1) is 0.05
～2.5mol/L.
5. method according to claim 1, it is characterised in that the washing described in step (2), is the solid for obtaining centrifugation
Jing absolute ethanol washings 2～3 times successively, deionized water are cleaned 1～3 time.
6. the method that a kind of utilization metallic tin according to claim 1 directly prepares tin oxide nano particles, its feature
It is, obtained tin oxide nano particles, by the nanoparticle of a diameter of 10～50nm with monodispersed form or certain journey
The aggregate form of degree is present, and can be adjusted according to experiment condition.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510860093.XA CN105293571B (en) | 2015-11-30 | 2015-11-30 | A kind of method that utilization metallic tin directly prepares tin oxide nano particles |
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| CN201510860093.XA CN105293571B (en) | 2015-11-30 | 2015-11-30 | A kind of method that utilization metallic tin directly prepares tin oxide nano particles |
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| CN105293571A CN105293571A (en) | 2016-02-03 |
| CN105293571B true CN105293571B (en) | 2017-03-29 |
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| CN113084717B (en) * | 2021-04-08 | 2022-05-03 | 华侨大学 | Porous Cu-Sn-based ultrathin grinding wheel for cutting chip and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1260133C (en) * | 2003-03-14 | 2006-06-21 | 中国科学院上海硅酸盐研究所 | Method for preparing nano tin-oxide powder |
| EP2038899A4 (en) * | 2006-06-06 | 2015-05-20 | Cornell Res Foundation Inc | Nanostructured metal oxides comprising internal voids and methods of use thereof |
| KR100850008B1 (en) * | 2007-05-07 | 2008-08-01 | 희성금속 주식회사 | A manufacturing method of nano particle tin oxide using surface catalyst reaction |
| CN101696029B (en) * | 2009-10-14 | 2011-05-11 | 大连交通大学 | Method for directly synthesizing liquid phase of tin oxide nano powder |
| CN102491407A (en) * | 2011-11-11 | 2012-06-13 | 上海交通大学 | Preparation method of tin dioxide nano material with controllable morphology |
| CN103848456A (en) * | 2012-12-05 | 2014-06-11 | 中国科学院理化技术研究所 | Preparation method of hollow stannic oxide micro-nano particles |
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Inventor after: Ji Yanyan Inventor after: Zhao Bo Inventor after: Deng Xuan Inventor after: Liu Qiang Inventor after: Li Jiang Inventor after: Zhao Hongyong Inventor before: Ji Yanyan Inventor before: Zhao Bo Inventor before: Deng Xuan Inventor before: Liu Qiang Inventor before: Li Jiang |
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