CN101372353A - Method for preparing nano CeO2 power by ultrasonic atomization process - Google Patents
Method for preparing nano CeO2 power by ultrasonic atomization process Download PDFInfo
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- CN101372353A CN101372353A CNA2008101239349A CN200810123934A CN101372353A CN 101372353 A CN101372353 A CN 101372353A CN A2008101239349 A CNA2008101239349 A CN A2008101239349A CN 200810123934 A CN200810123934 A CN 200810123934A CN 101372353 A CN101372353 A CN 101372353A
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Abstract
A method for preparing nano CeO2 powder by an ultrasonic atomization process relates to the preparation field of nano powder, and is characterized in that: a certain amount of cerium salt and a precipitant are respectively dissolved into distilled water to prepare a reaction solution with a certain concentration, wherein, the concentration range of Ce<3+> in the reaction solution is 0.1-1mol/L, and the concentration mol ratio of the precipitant to the cerium salt is 2:1-20: 1. The two reaction solutions are ultrasonically atomized respectively and introduced into a reactor for reaction after being mixed, and the suspended precipitate generated by the reaction is collected, washed, dried and calcined at the temperature of 300-800 DEG C for 0.5-3h to obtain the faint yellow nano CeO2 powder. The method has the advantages that the nano CeO2 powder with good monodispersion is prepared by a simple chemical process without complicated devices, a few cheap chemical raw materials with little pollution is needed, repeatability is good, and the shape of the particles is subsphaeroidal and the particle size thereof is nano grade.
Description
Technical field
The present invention relates to the nano powder preparation field, refer in particular to the ultrasonic atomizatio legal system be equipped with that monodispersity is good, the method for even particle size distribution, subsphaeroidal nano oxide powder.
Background technology
CeO
2As a kind of typical rare earth oxide many-sided functional performance is arranged, the intermediate materials, the membrane reactor material in the electrochemical cell, intermediate temperature solid oxide fuel cell (SOFC) that are widely used in electronic ceramics, radioresistive glass, luminescent material, catalytic material, chemically machinery polished (CMP) abrasive material, high temperature oxygen-sensitive material, pH sensing material, fuel cell have huge development potentiality with electrode materials etc. in the modern high technology field.Liquid phase method prepares superfine powder and has reaction conditions gentleness, easy to control, and the superfine powder that makes is formed evenly, the purity advantages of higher, thereby obtains broad research and application.Liquid phase method prepares nano Ce O
2Method mainly comprise: the precipitator method, sol-gel processing, hydrothermal method and microemulsion method etc.
But it is that particle agglomeration is serious, size-grade distribution is inhomogeneous, monodispersity is poor that traditional liquid phase method prepares nano-powder ubiquity problem, thereby has had a strong impact on the use properties of powder.Water/oil type microemulsion system that Mei Yan etc. utilize cetyl trimethyl ammonia bromide+propyl carbinol/hexanaphthene/aqueous solution to form is realized the microcell reaction, has prepared mono-dispersed nano CeO
2Particle, but this preparation process is too complicated, and the preparation cost height; Zhang Jiaqi etc. carry out pyrolysis later on the reaction solution ultrasonic atomizatio, have prepared the TiO of better performances
2Powder.At present, do not find to utilize ultrasonic atomizatio to realize microcell prepared in reaction nano Ce O as yet
2The relevant report of powder.
Summary of the invention
The present invention is a raw material with cerium salt, adopts that ultrasonic atomizatio technology synthesizing monodisperse is good, even particle size distribution, subsphaeroidal nano Ce O
2Powder.By optimizing cerium salt concn, cerium salt and precipitation agent concentration ratio, processing parameters such as calcination condition are controlled nano Ce O
2The pattern of powder and size-grade distribution, thus the subsphaeroidal nano Ce O of monodispersity obtained
2Powder.
Specific embodiment of the present invention is: take by weighing a certain amount of cerium salt and precipitation agent and be dissolved in respectively and be prepared into certain density reaction solution in the distilled water, wherein Ce in the reaction solution
3+Concentration range be 0.1～1mol/L, precipitation agent and cerium salt concn mol ratio are between 2:1～20:1.Mix afterreaction in the reactor that two kinds of reaction solns are fed behind the ultrasonic atomizatio respectively, and collect and react the suspension throw out that generates, with throw out washing, drying, pass through at last again, can obtain flaxen nano Ce O at 300 ℃～800 ℃ calcination 0.5～3h
2Powder.
Described cerium salt is any in cerous nitrate, cerous sulfate or the cerous carbonate;
Described precipitation agent be in bicarbonate of ammonia, sodium hydroxide or the ammoniacal liquor any.
The present invention adopts simple chemical technology to prepare the good nano Ce O of monodispersity
2Powder need not complex apparatus, and required chemical feedstocks kind is few, inexpensive, pollution is few, favorable repeatability, and its granule-morphology is subsphaeroidal, granularity is a nano level.
Description of drawings
Fig. 1 is for being raw material with cerous nitrate and bicarbonate of ammonia, wherein [Ce
3+]=0.4mol/l, bicarbonate of ammonia and cerous nitrate concentration mol ratio are 4:1, adopt the prepared nano Ce O of ultrasonic atomizatio technology
2Powder TEM photo.
Fig. 2 is for being raw material with cerous nitrate and bicarbonate of ammonia, wherein [Ce
3+]=0.1mol/l, bicarbonate of ammonia and cerous nitrate concentration mol ratio are 20:1, adopt the prepared nano Ce O of ultrasonic atomizatio technology
2Powder TEM photo.
Fig. 3 is for being raw material with cerous nitrate and sodium hydroxide, wherein [Ce
3+]=0.4mol/l, bicarbonate of ammonia and cerous nitrate concentration mol ratio are 3:1, adopt the prepared nano Ce O of ultrasonic atomizatio technology
2Powder TEM photo.
Fig. 4 is for being raw material with cerous nitrate and ammoniacal liquor, wherein [Ce
3+]=0.4mol/l, sodium hydroxide and cerous nitrate concentration mol ratio are 2:1, adopt the prepared nano Ce O of ultrasonic atomizatio technology
2Powder TEM photo.
Fig. 5 is for being raw material with cerous sulfate and bicarbonate of ammonia, wherein [Ce
3+]=0.5mol/l, sodium hydroxide and cerous nitrate concentration mol ratio are 4:1, adopt the prepared nano Ce O of ultrasonic atomizatio technology
2Powder TEM photo.
Fig. 6 is for being raw material with cerous carbonate and bicarbonate of ammonia, wherein [Ce
3+]=1mol/l, sodium hydroxide and cerous nitrate concentration mol ratio are 10:1, adopt the prepared nano Ce O of ultrasonic atomizatio technology
2Powder TEM photo.
Embodiment
The present invention is described in further detail below in conjunction with embodiment:
Embodiment 1:
Preparation Ce (NO
3)
3With each 200ml of ammonium bicarbonate soln, wherein [Ce
3+]=0.4mol/l, bicarbonate of ammonia and cerous nitrate concentration mol ratio are that 4:1 places ultrasonic atomizing device to atomize respectively two kinds of reaction solns, to react in the feeding of the reaction solution after the atomizing reactor, and will collect in the suspension throw out introducing collector that generate, obtain suspension liquid, obtain throw out by centrifugation again.With throw out distilled water wash three times, absolute ethanol washing one time is put into air dry oven and is dried, and through 300 ℃ of calcining 2h, obtains nano Ce O again
2Powder.
The CeO that makes by the processing parameter of embodiment 1
2The TEM photo of powder sample as shown in Figure 1, therefrom as can be seen, prepared CeO
2Diameter of particle is evenly distributed, and is closely spherical, and particle diameter calculates its population mean according to statistics and is about 3.8nm between 3～5nm.
Embodiment 2:
Change solution parameter preparation [Ce
3+] be 0.1mol/l, bicarbonate of ammonia and cerous nitrate concentration mol ratio are 20:1.Place ultrasonic atomizing device to atomize respectively two kinds of reaction solns, the reaction solution after the atomizing is fed in the reactor react, and, obtain suspension liquid, obtain throw out by centrifugation again collecting in the suspension throw out introducing collector that generates.With throw out distilled water wash three times, absolute ethanol washing one time is put into air dry oven and is dried, and through 300 ℃ of calcining 2h, obtains nano Ce O again
2Powder.
The CeO that makes by the processing parameter of embodiment 2
2The TEM photo of powder sample as shown in Figure 2.
Embodiment 3:
With sodium hydroxide is precipitation agent, changes solution parameter [Ce
3+] be 0.4mol/l, sodium hydroxide and cerous nitrate concentration mol ratio are 3:1.Place ultrasonic atomizing device to atomize respectively two kinds of reaction solns, the reaction solution after the atomizing is fed in the reactor react, and, obtain suspension liquid, obtain throw out by centrifugation again collecting in the suspension throw out introducing collector that generates.With throw out distilled water wash three times, absolute ethanol washing one time is put into air dry oven and is dried, and through 300 ℃ of calcining 2h, obtains nano Ce O again
2Powder.
The CeO that makes by the processing parameter of embodiment 3
2The TEM photo of powder sample as shown in Figure 3.
Embodiment 4:
With ammoniacal liquor is precipitation agent, changes solution parameter [Ce
3+] be 0.4mol/l, ammoniacal liquor and cerous nitrate concentration mol ratio are 2:1.Place ultrasonic atomizing device to atomize respectively two kinds of reaction solns, the reaction solution after the atomizing is fed in the reactor react, and, obtain suspension liquid, obtain throw out by centrifugation again collecting in the suspension throw out introducing collector that generates.With throw out distilled water wash three times, absolute ethanol washing one time is put into air dry oven and is dried, and through 300 ℃ of calcining 2h, obtains nano Ce O again
2Powder.
The CeO that makes by the processing parameter of embodiment 4
2The TEM photo of powder sample as shown in Figure 4.
Embodiment 5:
With the cerous sulfate is cerium salt, changes solution parameter [Ce
3+] be 0.5mol/l, bicarbonate of ammonia and cerous sulfate concentration mol ratio are 4:1.Place ultrasonic atomizing device to atomize respectively two kinds of reaction solns, the reaction solution after the atomizing is fed in the reactor react, and, obtain suspension liquid, obtain throw out by centrifugation again collecting in the suspension throw out introducing collector that generates.With throw out distilled water wash three times, absolute ethanol washing one time is put into air dry oven and is dried, and through 600 ℃ of calcining 1h, obtains nano Ce O again
2Powder.
The CeO that makes by the processing parameter of embodiment 5
2The TEM photo of powder sample as shown in Figure 5.
Embodiment 6:
With the cerous carbonate is cerium salt, changes solution parameter [Ce
3+] be 1mol/l, bicarbonate of ammonia and cerous carbonate concentration mol ratio are 10:1.Place ultrasonic atomizing device to atomize respectively two kinds of reaction solns, the reaction solution after the atomizing is fed in the reactor react, and, obtain suspension liquid, obtain throw out by centrifugation again collecting in the suspension throw out introducing collector that generates.With throw out distilled water wash three times, absolute ethanol washing one time is put into air dry oven and is dried, and through 800 ℃ of calcining 0.5h, obtains nano Ce O again
2Powder.
The CeO that makes by the processing parameter of embodiment 6
2The TEM photo of powder sample as shown in Figure 6.
Claims (1)
1. ultrasonic atomizatio prepared nano Ce O
2The method of powder is characterized in that taking by weighing a certain amount of cerium salt and precipitation agent and is dissolved in respectively and is prepared into certain density reaction solution in the distilled water, wherein Ce in the reaction solution
3+Concentration range be 0.1～1.0mol/L, precipitation agent and cerium salt concn mol ratio are between 2:1～20:1; Mix afterreaction in the reactor that two kinds of reaction solns are fed behind the ultrasonic atomizatio respectively, and collect and react the suspension throw out that generates, with throw out washing, drying, pass through at last again, can obtain flaxen nano Ce O at 300 ℃～800 ℃ calcination 0.5～3h
2Powder; Described cerium salt is any in cerous nitrate, cerous sulfate or the cerous carbonate; Described precipitation agent be in bicarbonate of ammonia, sodium hydroxide or the ammoniacal liquor any.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491490A (en) * | 2011-12-06 | 2012-06-13 | 江南大学 | Ozonated water treatment method with nano ceria as catalyst |
| CN103539194A (en) * | 2013-09-25 | 2014-01-29 | 西安迈克森新材料有限公司 | Method for preparing flake cerium carbonate |
| CN103818943A (en) * | 2014-02-18 | 2014-05-28 | 常州大学 | Spherical cerium oxide porous abrasive and its use in ultra-precision polishing |
| CN104843763A (en) * | 2015-05-26 | 2015-08-19 | 西安科技大学 | Preparation method for nanoparticle by ultrasonic spraying |
| CN106044829A (en) * | 2016-05-25 | 2016-10-26 | 南昌大学 | Preparation method of white pure cerium oxide |
| CN111689478A (en) * | 2020-06-11 | 2020-09-22 | 黄湛明 | Preparation method and preparation system of high-purity nano selenium powder |
| CN112158883A (en) * | 2020-10-16 | 2021-01-01 | 成都先进金属材料产业技术研究院有限公司 | Process for preparing vanadium dioxide nano powder |
| CN113120940A (en) * | 2019-12-30 | 2021-07-16 | 安集微电子科技（上海）股份有限公司 | Spherical cerium carbonate and synthesis method of cerium oxide |
| CN115064712A (en) * | 2022-08-03 | 2022-09-16 | 盐城工学院 | Preparation method of nanoparticle-coated composite cathode material |
| CN115445599A (en) * | 2022-09-26 | 2022-12-09 | 常州大学 | Honeycomb catalyst prepared by ultrasonic double-atomization method and application of honeycomb catalyst in catalytic oxidation degradation of VOCs |
| CN116332224A (en) * | 2023-03-22 | 2023-06-27 | 广东长信精密设备有限公司 | Spherical gallium oxide and preparation process thereof |
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2008
- 2008-06-12 CN CNA2008101239349A patent/CN101372353A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491490A (en) * | 2011-12-06 | 2012-06-13 | 江南大学 | Ozonated water treatment method with nano ceria as catalyst |
| CN103539194A (en) * | 2013-09-25 | 2014-01-29 | 西安迈克森新材料有限公司 | Method for preparing flake cerium carbonate |
| CN103818943A (en) * | 2014-02-18 | 2014-05-28 | 常州大学 | Spherical cerium oxide porous abrasive and its use in ultra-precision polishing |
| CN103818943B (en) * | 2014-02-18 | 2016-05-04 | 常州大学 | A kind of spherical cerium oxide porous abrasive and the purposes in Ultraprecise polished thereof |
| CN104843763A (en) * | 2015-05-26 | 2015-08-19 | 西安科技大学 | Preparation method for nanoparticle by ultrasonic spraying |
| CN106044829A (en) * | 2016-05-25 | 2016-10-26 | 南昌大学 | Preparation method of white pure cerium oxide |
| CN106044829B (en) * | 2016-05-25 | 2018-03-23 | 南昌大学 | A kind of preparation method of white pure zirconia cerium |
| CN106044829B8 (en) * | 2016-05-25 | 2018-11-27 | 赣州湛海工贸有限公司 | A kind of preparation method of white pure zirconia cerium |
| CN113120940A (en) * | 2019-12-30 | 2021-07-16 | 安集微电子科技（上海）股份有限公司 | Spherical cerium carbonate and synthesis method of cerium oxide |
| CN111689478A (en) * | 2020-06-11 | 2020-09-22 | 黄湛明 | Preparation method and preparation system of high-purity nano selenium powder |
| CN111689478B (en) * | 2020-06-11 | 2022-01-28 | 黄湛明 | Preparation method and preparation system of high-purity nano selenium powder |
| CN112158883A (en) * | 2020-10-16 | 2021-01-01 | 成都先进金属材料产业技术研究院有限公司 | Process for preparing vanadium dioxide nano powder |
| CN115064712A (en) * | 2022-08-03 | 2022-09-16 | 盐城工学院 | Preparation method of nanoparticle-coated composite cathode material |
| CN115064712B (en) * | 2022-08-03 | 2023-11-17 | 盐城工学院 | Preparation method of nanoparticle coated composite cathode material |
| CN115445599A (en) * | 2022-09-26 | 2022-12-09 | 常州大学 | Honeycomb catalyst prepared by ultrasonic double-atomization method and application of honeycomb catalyst in catalytic oxidation degradation of VOCs |
| CN115445599B (en) * | 2022-09-26 | 2023-08-22 | 常州大学 | Honeycomb catalyst prepared by ultrasonic double atomization method and application of honeycomb catalyst in catalytic oxidative degradation of VOCs |
| WO2023241737A1 (en) * | 2022-09-26 | 2023-12-21 | 常州大学 | Honeycomb catalyst prepared by utilizing ultrasonic double-atomization method, and use of same for catalytic oxidative degradation of vocs |
| CN116332224A (en) * | 2023-03-22 | 2023-06-27 | 广东长信精密设备有限公司 | Spherical gallium oxide and preparation process thereof |
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