CN101205078A - Method for preparing cerium dioxide nano-tube - Google Patents
Method for preparing cerium dioxide nano-tube Download PDFInfo
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- CN101205078A CN101205078A CN 200610165548 CN200610165548A CN101205078A CN 101205078 A CN101205078 A CN 101205078A CN 200610165548 CN200610165548 CN 200610165548 CN 200610165548 A CN200610165548 A CN 200610165548A CN 101205078 A CN101205078 A CN 101205078A
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- cerium dioxide
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Abstract
The invention provides a method for preparing a cerium dioxide nano-tube, which relates to a nano-tube technique. The method takes soluble cerium salt as precursor and excess sodium hydroxide as precipitator, which react under alkaline condition and then are moved to a reaction kettle to be heated for 10 to 24 hours under temperature of 100 to 160 DEG C; the sediment is separated, washed and dried under room temperature after cooled to the room temperature; the sediment prepared is dispersed into 1 to 5 percent of oxydol solution for being treated for 1 to 2 hours under ultrasonic; then the cerium dioxide nano-tube is prepared after separating, washing and drying.The cerium dioxide nano-tube prepared by the method of the invention has the advantages of good homogeneity, simple preparation method, cheap and easy-acquiredraw material, simple and feasible preparation technique and low cost. The thickness of the cerium dioxide nano-tube ranges from 5 to 7 nm, and the inner diameter is 10-20nm.
Description
Technical field
The present invention relates to a kind of preparation method of cerium dioxide nano-tube.
Background technology
Nano ceric oxide (CeO
2) be a kind of cheapness and the extremely wide industrial raw material of purposes, can be used as the main body material of the oxygen ion conductor of Solid Oxide Fuel Cell (SOFO), be used for making the Solid Oxide Fuel Cell (SOFO) of title with " green energy resource of 21 century "; The rumbling compound that is widely used in luminescent material, glass, glass decolouring finings etc.; Aspect environmental protection, be used as the three-effect catalysis auxiliary agent; It also is the important composition composition in superconductor, gas sensor, the commercial catalysts.Cerium dioxide (the CeO that tube wall is thin, tube chamber is big
2) preparation of nano-tube material becomes a problem that presses for research, is subjected to increasing attention.
Summary of the invention
The object of the present invention is to provide a kind of uniform cerium dioxide (CeO
2) preparation method of nanotube, used hydrothermal synthesis method and ultrasonication, prepared cerium dioxide (CeO
2) good uniformity of nanotube, tube wall is thin, tube chamber is big.
For achieving the above object, technical solution of the present invention is:
A kind of preparation method of cerium dioxide nano-tube:
Getting solubility cerium salt and sodium hydroxide is dissolved in respectively in an amount of water, sodium hydroxide solution is poured in the solubility cerium solution fast, and constantly stir till generating yellow mercury oxide, then it is transferred in the reactor, be put in the thermostat container and heat, the throw out that obtains with washed with de-ionized water after at room temperature dry 24h; Then these dry things are dispersed in 1～10% the hydrogen peroxide solution, under ultrasonic wave, handle 1～2h; The product of handling is obtained cerium dioxide nano-tube with the washed with de-ionized water after drying.
Described preparation method, its described solubility cerium salt is cerous sulfate, its concentration is 0.1～0.3mol/L.
Described preparation method, its described concentration of sodium hydroxide solution is at 1～10mol/L
Described preparation method heats in its described thermostat container, and temperature range is 100～160 ℃, and be 10～24h heat-up time.
Described preparation method, its described hydro-thermal reaction, temperature are preferably 100～160 ℃.
Described preparation method, the drying temperature of its described hydrothermal product is a room temperature.
Described preparation method, its described hydrogen peroxide concentration is 1～5%.
The cerium dioxide nano-tube homogeneity that the inventive method prepares is good, and the preparation method is simple, thickness of pipe 5～7nm, and bore is 10～20nm, and starting material are cheap and easy to get, and preparation is simple, with low cost.
Description of drawings
Fig. 1 is the XRD figure spectrum of oxide compound shown in the embodiment 1;
Fig. 2 is transmission electron microscope (TEM) the pattern photo of embodiment 1;
Fig. 3 is transmission electron microscope (TEM) the pattern photo of embodiment 2;
Fig. 4 is transmission electron microscope (TEM) the pattern photo of embodiment 3;
Fig. 5 is transmission electron microscope (TEM) the pattern photo of embodiment 4.
Embodiment
It is the cerium source that method provided by the invention adopts the cerous sulfate of solubility, be dissolved in wiring solution-forming in a certain amount of water, prepare sodium hydroxide solution in addition, with two solution hybrid reactions and continuous the stirring till the xanchromatic throw out, then it is transferred to and puts into the thermostat container thermostatically heating in the reactor, the throw out that obtains is at room temperature dry after with washed with de-ionized water.Then these dry things are dispersed in 1～10% the hydrogen peroxide solution, under ultrasonic wave, handled 1～2 hour.Product is obtained cerium dioxide nano-tube with the washed with de-ionized water after drying.
The invention provides the above-mentioned nano ceric oxide (CeO of preparation
2) method of cubic block, its key step is as follows:
A) preparation cerous sulfate solution, concentration is controlled at 0.1～0.3mol/L;
B) preparation sodium hydroxide solution, concentration is controlled at 1～10mol/L;
C) solution that step b is obtained joins in the solution that a step obtains rapidly, and constantly stirs, till throw out occurring;
D) the throw out mixed solution that step c is obtained is transferred to reactor, and it is transferred to thermostat container, at 100～160 ℃ of following thermostatically heating 10～24h;
E) the product deionized water wash that steps d is obtained, at room temperature dry;
F) product that step e is obtained is dispersed in 1～5% the hydrogen peroxide solution, handles 1h～2h under ultrasonic wave;
G) the product deionized water wash that step f is obtained promptly obtains cerium dioxide (CeO after the drying
2) nanotube.
Embodiment 1: claim Ce
2(SO
4)
39H
2O 1.5g is dissolved in the 10ml deionized water, obtains solution 1.Other takes by weighing NaOH4.8g, is dissolved in the 30ml deionized water, obtains solution 2.Solution 2 is joined rapidly in the solution 1, and continuous the stirring till generating throw out, transfer to then to be put in the reactor in the thermostat container and heat 12h down at 110 ℃, with the throw out that obtains deionized water wash, dry 24h under 20 ℃.Desciccate is dispersed in 5% the hydrogen peroxide, under ultrasonic wave, handles 1h.Product is separated, and washing obtains CeO after the drying
2Nanotube.
Embodiment 2: difference from Example 1 is that the temperature of the heating in thermostat container is 130 ℃, and all the other steps are with embodiment 1.
Embodiment 3: difference from Example 2 is, is 1.5h in the following treatment time of ultrasonic wave, and all the other steps are with embodiment 2.
Embodiment 4: difference from Example 2 is, is 2h in the following treatment time of ultrasonic wave, and all the other steps are with embodiment 2.
See Fig. 1, from the test result of sample X-ray diffraction (XRD), the sample characteristic diffraction peak that the present invention makes is CeO
2Crystalline phase.See Fig. 2～5, cerium dioxide nano-tube transmission electron microscope (TEM) the pattern photo of the inventive method preparation shows gained CeO
2Material is a nanotube, and thickness of pipe 5～7nm, bore are 10～20nm.
Claims (7)
1. the preparation method of a cerium dioxide nano-tube is characterized in that:
Getting solubility cerium salt and sodium hydroxide is dissolved in respectively in an amount of water, sodium hydroxide solution is poured in the solubility cerium solution fast, and constantly stir till generating yellow mercury oxide, then it is transferred in the reactor, be put in the thermostat container and heat, carry out hydro-thermal reaction, the throw out-hydrothermal product that obtains is with at room temperature dry 24h after the washed with de-ionized water; Then these dry things are dispersed in 1～10% the hydrogen peroxide solution, under ultrasonic wave, handle 1～2h; The product of handling is obtained cerium dioxide nano-tube with the washed with de-ionized water after drying.
2. preparation method according to claim 1 is characterized in that, described solubility cerium salt is cerous sulfate, and its concentration is 0.1～0.3mol/L.
3. preparation method according to claim 1 is characterized in that described concentration of sodium hydroxide solution is at 1～10mol/L.
4. preparation method according to claim 1 is characterized in that, heats in the described thermostat container, and temperature range is 100～160 ℃, and be 10～24h heat-up time.
5. preparation method according to claim 1 is characterized in that, described hydro-thermal reaction, temperature are preferably 100～160 ℃.
6. preparation method according to claim 1 is characterized in that, the drying temperature of described hydrothermal product is a room temperature.
7. preparation method according to claim 1 is characterized in that, described hydrogen peroxide concentration is 1～5%.
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| CN2006101655487A CN101205078B (en) | 2006-12-21 | 2006-12-21 | Method for preparing cerium dioxide nano-tube |
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| CN2006101655487A CN101205078B (en) | 2006-12-21 | 2006-12-21 | Method for preparing cerium dioxide nano-tube |
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| CN101205078B CN101205078B (en) | 2010-06-09 |
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Cited By (9)
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| CN101824745A (en) * | 2010-04-12 | 2010-09-08 | 江苏工业学院 | Method for preparing anti-UV fabric by in-situ method |
| CN101920984A (en) * | 2010-08-11 | 2010-12-22 | 中国科学院合肥物质科学研究院 | Method for preparing mesoporous CeO2 nano-tubes having large specific surface area and high catalytic activity |
| CN101669881B (en) * | 2009-08-17 | 2011-08-03 | 李榕卿 | Dental material containing rare earth elements |
| CN106495202A (en) * | 2016-11-10 | 2017-03-15 | 中国科学院上海高等研究院 | Rare earth metal hydroxide and oxide porous tunnel nanotube and preparation method |
| CN107651703A (en) * | 2017-09-19 | 2018-02-02 | 天津大学 | The preparation method of particular crystal plane nano ceric oxide |
| CN110422871A (en) * | 2019-08-20 | 2019-11-08 | 南昌大学 | The preparation method of Cerium Oxide Nanotubes |
| CN114368773A (en) * | 2021-12-09 | 2022-04-19 | 江西师范大学 | Method for preparing cerium dioxide nano particles by two-step method |
| CN114620755A (en) * | 2021-12-30 | 2022-06-14 | 南京大学 | Cerium dioxide nanotube and preparation method thereof |
| CN114702059A (en) * | 2021-12-30 | 2022-07-05 | 南京大学 | Binary hydroxide nanotube with composite structure and preparation method thereof |
Families Citing this family (1)
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| UA102627C2 (en) | 2012-03-20 | 2013-07-25 | Общество С Ограниченной Ответственностью "Наномедтраст" | Nanocomposite of cerium oxide-aluminosilicate tubes and process for the preparation thereof |
Family Cites Families (3)
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| JP2000203834A (en) * | 1998-12-28 | 2000-07-25 | Kose Corp | Ultrafine cerium oxide particle and ultrafine metal oxide.cerium oxide particle, its production and resin composition and cosmetic containing the same |
| JP4214028B2 (en) * | 2003-09-30 | 2009-01-28 | 大王製紙株式会社 | Absorbent packaging structure |
| CN1242922C (en) * | 2004-01-09 | 2006-02-22 | 山东师范大学 | Synthesis method of cerium oxide nano material |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101669881B (en) * | 2009-08-17 | 2011-08-03 | 李榕卿 | Dental material containing rare earth elements |
| CN101824745A (en) * | 2010-04-12 | 2010-09-08 | 江苏工业学院 | Method for preparing anti-UV fabric by in-situ method |
| CN101920984A (en) * | 2010-08-11 | 2010-12-22 | 中国科学院合肥物质科学研究院 | Method for preparing mesoporous CeO2 nano-tubes having large specific surface area and high catalytic activity |
| CN106495202A (en) * | 2016-11-10 | 2017-03-15 | 中国科学院上海高等研究院 | Rare earth metal hydroxide and oxide porous tunnel nanotube and preparation method |
| CN106495202B (en) * | 2016-11-10 | 2018-03-02 | 中国科学院上海高等研究院 | Rare earth metal hydroxide and oxide porous tunnel nanotube and preparation method |
| CN107651703A (en) * | 2017-09-19 | 2018-02-02 | 天津大学 | The preparation method of particular crystal plane nano ceric oxide |
| CN110422871A (en) * | 2019-08-20 | 2019-11-08 | 南昌大学 | The preparation method of Cerium Oxide Nanotubes |
| CN114368773A (en) * | 2021-12-09 | 2022-04-19 | 江西师范大学 | Method for preparing cerium dioxide nano particles by two-step method |
| CN114620755A (en) * | 2021-12-30 | 2022-06-14 | 南京大学 | Cerium dioxide nanotube and preparation method thereof |
| CN114702059A (en) * | 2021-12-30 | 2022-07-05 | 南京大学 | Binary hydroxide nanotube with composite structure and preparation method thereof |
| CN114620755B (en) * | 2021-12-30 | 2023-09-05 | 南京大学 | Cerium dioxide nanotube and preparation method thereof |
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| CN101205078B (en) | 2010-06-09 |
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