CN101298338A - Electron beam radiation synthetic method of stannic oxide nano-rod - Google Patents
Electron beam radiation synthetic method of stannic oxide nano-rod Download PDFInfo
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- CN101298338A CN101298338A CNA2008100363955A CN200810036395A CN101298338A CN 101298338 A CN101298338 A CN 101298338A CN A2008100363955 A CNA2008100363955 A CN A2008100363955A CN 200810036395 A CN200810036395 A CN 200810036395A CN 101298338 A CN101298338 A CN 101298338A
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Abstract
The invention relates to an electron-beam irradiation synthetic method for a tin dioxide nanometer rod crystal, which belongs to the technical field of nanometer inorganic compound semiconductor material. The methof of the invention adopts the tin tetrachloride as raw material, a certain amount of surface-active material polyvinyl alcohol is added with the volume ratio of 100:3-100:5, then a diluted sodium hydroxide is added after the solution is stirred uniformly by magnetic power, the PH value is adjusted to 8-10, then the solution is placed into a sealed container and is put under the electron beam emitted by a 2.0 MeV, 10mA electron accelerator for irradiation treatment, the irradiation dose is set as 250-400 KGy and the irradiation period is 5-10 hours, and finally the white tin dioxide nanometer rod microcrystal material is obtained after the washing, centrifugal separation and drying process. The material has good gas-sensitive characteristics and the method of the invention has simple synthesis technique and can produce under the normal temperature and pressure without any catalyst.
Description
Technical field
The present invention relates to a kind of electronic-beam radiation synthesizing method of nanometer tin dioxide rod, belong to nm inorganic compound semiconductor material manufacturing process technology field.
Background technology
Tindioxide is a kind of important semiconductor material, has broad energy gap (Eg=3.6eV), and it is extensive to have raw material sources, advantages such as low price.Tindioxide is prepared into size when tens nanometers are following, because small-size effect and surface effects, make it have special photoelectric properties and air-sensitive performance, not only have a wide range of applications (being to be applied in one of maximum basic raw material of gas sensor at present) fields such as also can be used for electrode materials, dog sun can battery, opto-electronic device, absorbing material at aspects such as air-sensitive, wet quick, optical technologies.For example, the gas sensor for preparing with nano level tindioxide has characteristics such as highly sensitive, that working temperature is low, the time of response is short, is widely used in the detection of reducing gas or toxic gas.With nano level tindioxide as the new type lithium ion battery negative material, because the particle of tindioxide is a nano level, also nano-scale between particle voids, for the embedding of lithium ion provides good nanochannel and embedding lithium position, have big embedding lithium capacity and embedding lithium performance, under the charge status of big electric current, still has bigger reversible capacity.
The method of the at present existing nano level tindioxide of multiple preparation comprises chemical Vapor deposition process, chemical precipitation method, sol-gel method, hydro-thermal solvent method etc.But complex process is arranged, and preparation time is long, the more high shortcoming of cost.Adopt gamma-rays radiation method irradiation technique to prepare the method that nano material is a kind of novelty, but also can produce radwaste, technical process is an intermittent type, can not continuous production etc. shortcoming.
Summary of the invention
The electronic-beam radiation synthesizing method that the purpose of this invention is to provide a kind of nano-stannic oxide semiconductor material.
A kind of nanometer tin dioxide rod crystalline electronic-beam radiation synthesizing method of the present invention is characterized in that following process and step are arranged:
A. polyvinyl alcohol is mixed with mass percent concentration and is 5～10% the aqueous solution; It is 3～6% the aqueous solution that tin tetrachloride is mixed with mass percent concentration; In above-mentioned tin tetrachloride solution, add above-mentioned polyvinyl alcohol solution then;
The used tin tetrachloride solution and the nominal mix proportion of polyvinyl alcohol solution are 100: 3～100: 5; Stirred 5～10 minutes, and regulated pH value to 8～10 of mixing solutions then;
B. will carry out radiation treatment after the above-mentioned mixing solutions sealing, its irradiation dose is to place behind 250～400KGy irradiation 5～10 hours;
C. use the above-mentioned resultant of reaction behind irradiation of distilled water wash then, clean with ethanol again, and centrifugation, to remove wherein unreacted ion and polyvinyl alcohol;
D. the resultant after will cleaning is dried under 60～80 ℃ of temperature, final white nanometer tin dioxide rod.
The inventive method is in the irradiation process, the adding of surface active agent polyvinyl alcohol, can carry out surface modification to particle, cover one layer of polymeric at particle surface, so not only can control the growth of particle nucleation, and can prevent solution evaporation the time because the high superficiality of atoms metal particulate, high chemical energy and the particle aggregation phenomenon that takes place, behind the irradiation, the tin dioxide nano-particle that generates hydroxyl on high-power electron beam effect lower surface generation defective and polyvinyl alcohol molecule has stronger reactive force, in put procedure, the hydroxyl self-assembly generates nanometer tin dioxide rod on the polyvinyl alcohol molecule.
The prepared nanometer tin dioxide rod crystallite of the inventive method has good dispersiveness.This nano bar-shape crystal shows good air-sensitive performance in the sensing capabilities test.
Advantage of the present invention is not use any catalyzer just can make under the normal temperature routine.In addition, synthesis technique of the present invention is simple, and is with low cost.Because adopt electron beam irradiation, electron beam is produced by rumbatron, rumbatron cuts out, and electron beam disappears immediately, so security is good, and pollution-free, help environmental protection.
Description of drawings
Fig. 1 is the prepared SnO of electron beam irradiation of the present invention
2Nanocrystalline X-ray diffraction analysis (XRD) collection of illustrative plates.
Fig. 2 is the prepared nanometer tin dioxide rod crystalline of the inventive method transmission electron microscope (TEM) photo figure.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1
The concrete preparation process of present embodiment is as follows:
(1) at first, take by weighing a certain amount of polyvinyl alcohol (PVA) with electronic balance, the configuration quality percentage concentration is 5% the aqueous solution; Take by weighing a certain amount of tin tetrachloride configuration quality percentage concentration again and be 3% aqueous solution 100ml; In tin tetrachloride solution, add 5ml PVA then, and, solution is mixed with magnetic stirrer 5 minutes; And then the dropping diluted sodium hydroxide solution is adjusted to 10 with the pH value;
(2) sealed vessel that the above-mentioned mixing solutions for preparing will be housed is positioned under the electron beam that rumbatron produces and carries out radiation treatment, and the energy of rumbatron accelerated electron is 2.0MeV, and the sub-line amount of purport intensity is 10mA, and its irradiation dose is 250KGy; The product that the irradiation afterreaction generates was placed 5 hours;
(3) use the above-mentioned resultant of reaction behind irradiation of distilled water wash then, clean with ethanol, and use the supercentrifuge centrifugation, repeated multiple times is to remove wherein unreacted effect and hydrophilic surfactant polyvinyl alcohol;
(4) resultant of reaction is placed in the baking oven dryly, temperature is 60 ℃, and drying time is 10 hours, final white nanometer tin dioxide rod sample A.
Embodiment 2
The concrete preparation process of present embodiment is as follows:
(1) at first, take by weighing a certain amount of polyvinyl alcohol (PVA) with electronic balance, the configuration quality percentage concentration is 10% the aqueous solution; Take by weighing a certain amount of tin tetrachloride configuration quality percentage concentration again and be 6% aqueous solution 100ml; In tin tetrachloride solution, add 3ml PVA then, and, solution is mixed with magnetic stirrer 5 minutes; And then the dropping diluted sodium hydroxide solution is adjusted to 8 with the pH value;
(2) sealed vessel that the above-mentioned mixing solutions for preparing will be housed is positioned under the electron beam that rumbatron produces and carries out radiation treatment, and the energy of rumbatron accelerated electron is 2.0MeV, and the sub-line amount of purport intensity is 10mA, and its irradiation dose is 400KGy; The product that the irradiation afterreaction generates was placed 10 hours;
(3) use the above-mentioned resultant of reaction behind irradiation of distilled water wash then, clean with ethanol, and use the supercentrifuge centrifugation, repeated multiple times is to remove wherein unreacted effect and hydrophilic surfactant polyvinyl alcohol;
(4) resultant of reaction is placed in the baking oven dryly, temperature is 80 ℃, and drying time is 6 hours, final white nanometer tin dioxide rod sample B.
Every instrument detecting result is as follows:
1, use X-ray diffraction analysis (XRD) test result referring to Fig. 1, as we know from the figure, the diffraction peak among the figure can determine that the white powder sample A of above-mentioned two embodiment gained and sample B are equal tetragonal structure nano-stannic oxide.
2, observe with transmission electron microscope (TEM), referring to Fig. 2, visible its length of prepared nanometer tin dioxide rod is about 200nm from this photo, and width is 40～50nm.
3, be assembled into the former film air-sensitive of tindioxide test element by material, test it respectively, record its sensitivity and be respectively 5.1 and 8.6, show good gas-sensitive property the formaldehyde of 50ppm, the sensitivity of methyl alcohol with sample A and sample B.This material is suitable as gas sensitive and detects reducing gas and toxic gas.
Claims (1)
1. nanometer tin dioxide rod crystalline electronic-beam radiation synthesizing method is characterized in that following process and step are arranged:
A. polyvinyl alcohol is mixed with mass percent concentration and is 5～10% the aqueous solution; It is 3～6% the aqueous solution that tin tetrachloride is mixed with mass percent concentration; In above-mentioned tin tetrachloride solution, add above-mentioned polyvinyl alcohol solution then;
The used tin tetrachloride solution and the nominal mix proportion of polyvinyl alcohol solution are 100: 3～100: 5; Stirred 5～10 minutes, and regulated pH value to 8～10 of mixing solutions then;
B. will carry out radiation treatment after the above-mentioned mixing solutions sealing, its irradiation dose is 250～400KGy; Placed behind the irradiation 5～10 hours;
C. use the above-mentioned resultant of reaction behind irradiation of distilled water wash then, clean with ethanol again, and centrifugation, to remove wherein unreacted ion and polyvinyl alcohol;
D. the resultant after will cleaning is dried under 60～80 ℃ of temperature, final white nanometer tin dioxide rod.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102653414A (en) * | 2011-03-04 | 2012-09-05 | 中国科学院金属研究所 | Nano crystal grain tin dioxide electron beam preparation method |
| CN104528809A (en) * | 2015-01-14 | 2015-04-22 | 广州大学 | Photochemical preparation method of stannic oxide nano-rod |
| CN108593843A (en) * | 2018-04-17 | 2018-09-28 | 华南师范大学 | A kind of SnO2Nanotube gas sensitive and the preparation method and application thereof |
| CN111455410A (en) * | 2020-02-28 | 2020-07-28 | 东南大学 | Method for preparing lithium-tin alloy nanocrystals by electron beam irradiation |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100367029C (en) * | 2005-06-16 | 2008-02-06 | 广州大学 | Stannic oxide based nanometer rod air-sensitive material and process for preparing the same |
| CN100410655C (en) * | 2005-07-05 | 2008-08-13 | 广州大学 | Tin-dioxide-base composite nano air-sensitive material and preparation method thereof |
-
2008
- 2008-04-21 CN CN2008100363955A patent/CN101298338B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102653414A (en) * | 2011-03-04 | 2012-09-05 | 中国科学院金属研究所 | Nano crystal grain tin dioxide electron beam preparation method |
| CN102653414B (en) * | 2011-03-04 | 2013-10-09 | 中国科学院金属研究所 | Nano crystal grain tin dioxide electron beam preparation method |
| CN104528809A (en) * | 2015-01-14 | 2015-04-22 | 广州大学 | Photochemical preparation method of stannic oxide nano-rod |
| CN104528809B (en) * | 2015-01-14 | 2017-01-18 | 广州大学 | Photochemical preparation method of stannic oxide nano-rod |
| CN108593843A (en) * | 2018-04-17 | 2018-09-28 | 华南师范大学 | A kind of SnO2Nanotube gas sensitive and the preparation method and application thereof |
| CN108593843B (en) * | 2018-04-17 | 2020-07-28 | 华南师范大学 | SnO (stannic oxide)2Nanotube gas-sensitive material and preparation method and application thereof |
| CN111455410A (en) * | 2020-02-28 | 2020-07-28 | 东南大学 | Method for preparing lithium-tin alloy nanocrystals by electron beam irradiation |
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