CN102942204A - Method for preparing cerium dioxide nanometer powder - Google Patents
Method for preparing cerium dioxide nanometer powder Download PDFInfo
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- CN102942204A CN102942204A CN2012104732230A CN201210473223A CN102942204A CN 102942204 A CN102942204 A CN 102942204A CN 2012104732230 A CN2012104732230 A CN 2012104732230A CN 201210473223 A CN201210473223 A CN 201210473223A CN 102942204 A CN102942204 A CN 102942204A
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- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 title abstract description 5
- 238000000034 method Methods 0.000 title description 10
- 239000011858 nanopowder Substances 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract 5
- 239000000243 solution Substances 0.000 claims abstract 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract 2
- 229910002492 Ce(NO3)3·6H2O Inorganic materials 0.000 claims 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 15
- 239000000463 material Substances 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 12
- NSOXQYCFHDMMGV-UHFFFAOYSA-N Tetrakis(2-hydroxypropyl)ethylenediamine Chemical compound CC(O)CN(CC(C)O)CCN(CC(C)O)CC(C)O NSOXQYCFHDMMGV-UHFFFAOYSA-N 0.000 description 11
- 238000002156 mixing Methods 0.000 description 10
- 206010013786 Dry skin Diseases 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000002045 lasting effect Effects 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000000975 co-precipitation Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 241000167847 Koelreuteria paniculata Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- -1 ultraviolet screener Substances 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
一种二氧化铈纳米粉体的制备方法，将Ce(NO3)3·6H2O溶解于去离子水中得Ce(NO3)3溶液；将乙二胺、PVP、KBrO3加入Ce(NO3)3溶液中持续搅拌均匀得混合溶液；将混合溶液移入反应釜中，置于微波水热仪中于160～200℃反应0.5～1.5h，反应后离心洗涤，80℃干燥得到CeO2纳米粉体。本发明成本低，操作简单且易于控制，本发明中微波水热法制备CeO2纳米粉体可以直接应用于掺杂及复合CeO2纳米粉体的制备中，为CeO2基新材料制备的提供了一种新途径。此外相对于传统水热法，微波水热法具有环保节能高效的优点。A preparation method of ceria nanopowder, dissolving Ce(NO 3 ) 3 6H 2 O in deionized water to obtain Ce(NO 3 ) 3 solution; adding ethylenediamine, PVP, KBrO 3 into Ce(NO 3 ) 3 ) Stir continuously in the 3 solution to obtain a mixed solution; move the mixed solution into a reaction kettle, place the mixed solution in a microwave hydrothermal instrument at 160-200°C for 0.5-1.5h, centrifuge and wash after the reaction, and dry at 80°C to obtain CeO2nm Powder. The present invention is low in cost, simple in operation and easy to control, and the CeO2 nano-powder prepared by the microwave hydrothermal method in the present invention can be directly applied to the preparation of doping and composite CeO2 nano-powder, providing a basis for the preparation of CeO2- based new materials a new way. In addition, compared with the traditional hydrothermal method, the microwave hydrothermal method has the advantages of environmental protection, energy saving and high efficiency.
Description
Technical field
The present invention relates to a kind of preparation method of cerium dioxide, particularly a kind of preparation method of cerium dioxide nano powder.
Background technology
CeO
2Be a kind of important function rare earth oxide, have cubic crystal structure.CeO
2Have good electric property and optical property, have a wide range of applications at numerous areas such as automotive exhaust catalysis, photodissociation water, ultraviolet screener, gas sensor, fuel-cell electrolyte, polishing material, hydrogen-storing materials, have good prospect.Nano Ce O
2And matrix material has higher specific surface energy and oxygen storage capacity, has good catalytic performance.At catalytic field, CeO
2Usually carry out the catalyzer of compound common formation excellent property as carrier and metal, not only dispersion, plastotype and stable effect are played in the metal of institute's load, and its oxygen storage capacity can also provide active oxygen when carrying out catalyzed reaction, play the effect of associating catalysis with catalyst body, the status that its effect has surmounted the catalyst cupport body.CeO
2The oxygen room on surface can promptly form and eliminate, and surface C e occurs
4+/ Ce
3+Oxidation reduction cycle.In photocatalysis to degrade organic matter, Ce
4+With Ce
3+Between the simple composite of transition energy establishment electron-hole pair, improve photocatalysis efficiency.In addition, the specific surface area of catalyzer has vital role to absorption-catalytic efficiency.Therefore, its size has vital effect to the whole structure of catalyzer.
Up to now, people have used several different methods to prepare CeO
2And composite material nanometer material.The reverse coprecipitation method of the utilizations such as LinYue has prepared CeO
2And Dope nano-power [Lin Yue, Xiao-MingZhang.Structural characterization and photocatalytic behaviors of doped CeO
2Nanoparticles[J] .Journal of Alloy and Compounds, 475 (2009), 702-705].Qiu Kehui etc. adopt sol-gel (sol-gel) legal system for V take cerous nitrate, citric acid and ammonium meta-vanadate as raw material
5+Ion-doped nano CeO
2Powder [Qiu Kehui, Zhang Wei, Li Junfeng, Wang Kejia .V
5+Synthetic and the sign [J] of ion-doped nano cerium oxide. China rare earth journal, 2009.4 (27,2): 209-212].But, need calcining process in the preparation process such as coprecipitation method, sol-gel method and microemulsion method, thereby the powder reuniting of preparing is comparatively serious, the large and pattern of granularity is difficult to control, has affected its performance.The precious equality of goldenrain tree has been synthesized sphere as the cerium source by hydrothermal method take cerous nitrate, fusiform and bouquet shape cerium dioxide [Luan Baoping, Yu Xibin, Liu Jie, Wang Litong, Hua Qingsong, Zhou Xiang, the CeO of different-shape
2Hydrothermal method preparation and characterization [J]. Shanghai Normal University's journal (natural science edition), 2011,40,2:157-162].But low, the consuming time length of traditional hydrothermal method productive rate and energy consumption are high, are unfavorable for a large amount of productions.
The microwave hydrothermal synthesis method is the novel method for synthesizing that utilizes microwave that the dielectric effect of water is heated the U.S. R.Roy of University of Pennsylvania proposition in 1992, compare with traditional hydrothermal method, the microwave hydrothermal synthesis method have rate of heating fast, be quick on the draw, the characteristics such as system is heated evenly, can prepare fast the superfine powder of pattern homogeneous.
Summary of the invention
The object of the present invention is to provide a kind of cost low, the preparation method of the simple to operate and cerium dioxide nano powder that is easy to control.
For achieving the above object, the technical solution used in the present invention is:
Step 1: with analytically pure Ce (NO
3)
36H
2O is dissolved in and gets concentration in the deionized water is the Ce (NO of 0.01～0.2mol/L
3)
3Solution;
With quadrol, PVP, KBrO
3With Ce (NO
3)
36H
2O presses (1 ~ 4): (3 ~ 6): (3 ~ 5): 1 mol ratio is with quadrol, PVP, KBrO
3Add Ce (NO
3)
3Continue the mixing solutions that stirs to get in the solution;
Step 2: mixing solutions is moved in the reactor, place the microwave hydrothermal instrument in 160 ~ 200 ℃ of reaction 0.5 ~ 1.5h, centrifuge washing after the reaction, 80 ℃ of dryings obtain CeO
2Nano-powder.
Described lasting stirring is to continue to stir 2h at 60 ℃.
The present invention reports and has adopted microwave-hydrothermal method one-step synthesis CeO
2Nano-powder is with Ce (NO
3)
36H
2O, quadrol, KBrO
3, the PVP(polyvinylpyrrolidone) be raw material, adopt microwave-hydrothermal method to prepare mean sizes and be about CeO about 30nm
2Nano-powder.The distinctive advantage of this method is that raw material is relatively inexpensive, and technological operation is simple, adopts the microwave-hydrothermal method of pollution-free clean low power consuming to prepare fast CeO
2Nano-powder.These advantages make the method have the potentiality of industrialization.
Beneficial effect of the present invention is embodied in: cost is low, simple to operate and be easy to control, microwave-hydrothermal method prepares CeO among the present invention
2Nano-powder can directly apply to and mix and compound CeO
2In the preparation of nano-powder, be CeO
2The base fabrication of new materials a kind of new way is provided.With respect to traditional hydrothermal method, microwave-hydrothermal method has the advantage of environment protection energy-saving efficient in addition.
Description of drawings
Fig. 1 is the CeO of embodiment 1 preparation
2The XRD diffractogram of nano-powder;
Fig. 2 is the CeO of embodiment 1 preparation
2The stereoscan photograph of nano-powder.
Embodiment
Embodiment 1:
Step 1: with analytically pure Ce (NO
3)
36H
2O is dissolved in and gets concentration in the deionized water is the Ce (NO of 0.01mol/L
3)
3Solution;
With quadrol, PVP, KBrO
3With Ce (NO
3)
36H
2O presses the mol ratio of 2:4:3:1 with quadrol, PVP, KBrO
3Add Ce (NO
3)
360 ℃ of lasting 2h that stir get mixing solutions in the solution;
Step 2: mixing solutions is moved in the reactor, place the microwave hydrothermal instrument in 180 ℃ of reaction 0.5h, centrifuge washing after the reaction, 80 ℃ of dryings obtain CeO
2Nano-powder.
CeO with gained
2Nano-powder is measured with the Japanese Rigaku production D/Max-2200pc of company type X-ray diffractometer, and the result obtains preferably pure phase CeO of crystallinity as shown in Figure 1
2Nano-powder finds that the JCPDS card number of product is 33-0394, belongs to isometric system.The microscopic appearance of this sample adopts HITACHI S4800 type scanning electronic microscope to observe, and the result is Fig. 2, and as can be seen from the figure that prepared is CeO
2Nano-powder, its mean sizes is approximately 30nm.
Embodiment 2:
Step 1: with analytically pure Ce (NO
3)
36H
2O is dissolved in and gets concentration in the deionized water is the Ce (NO of 0.05mol/L
3)
3Solution;
With quadrol, PVP, KBrO
3With Ce (NO
3)
36H
2O presses the mol ratio of 4:3:5:1 with quadrol, PVP, KBrO
3Add Ce (NO
3)
360 ℃ of lasting 2h that stir get mixing solutions in the solution;
Step 2: mixing solutions is moved in the reactor, place the microwave hydrothermal instrument in 160 ℃ of reaction 1.5h, centrifuge washing after the reaction, 80 ℃ of dryings obtain CeO
2Nano-powder.
Embodiment 3:
Step 1: with analytically pure Ce (NO
3)
36H
2O is dissolved in and gets concentration in the deionized water is the Ce (NO of 0.1mol/L
3)
3Solution;
With quadrol, PVP, KBrO
3With Ce (NO
3)
36H
2O presses the mol ratio of 1:6:4:1 with quadrol, PVP, KBrO
3Add Ce (NO
3)
360 ℃ of lasting 2h that stir get mixing solutions in the solution;
Step 2: mixing solutions is moved in the reactor, place the microwave hydrothermal instrument in 190 ℃ of reaction 1h, centrifuge washing after the reaction, 80 ℃ of dryings obtain CeO
2Nano-powder.
Embodiment 4:
Step 1: with analytically pure Ce (NO
3)
36H
2O is dissolved in and gets concentration in the deionized water is the Ce (NO of 0.2mol/L
3)
3Solution;
With quadrol, PVP, KBrO
3With Ce (NO
3)
36H
2O presses the mol ratio of 3:5:4:1 with quadrol, PVP, KBrO
3Add Ce (NO
3)
360 ℃ of lasting 2h that stir get mixing solutions in the solution;
Step 2: mixing solutions is moved in the reactor, place the microwave hydrothermal instrument in 200 ℃ of reaction 1h, centrifuge washing after the reaction, 80 ℃ of dryings obtain CeO
2Nano-powder.
Claims (2)
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|---|---|---|---|
| CN2012104732230A CN102942204A (en) | 2012-11-20 | 2012-11-20 | Method for preparing cerium dioxide nanometer powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI607969B (en) * | 2014-09-12 | 2017-12-11 | 台灣積體電路製造股份有限公司 | Method for manufacturing cerium dioxide powders and cerium dioxide powders |
| CN109438010A (en) * | 2018-11-29 | 2019-03-08 | 盛世生态环境股份有限公司 | A method of compost is prepared using garden waste and breeding wastewater |
| CN111579515A (en) * | 2020-05-26 | 2020-08-25 | 山东理工大学 | A method for oxidizing TMB with nano-cerium dioxide as simulated oxidase |
| CN115465879A (en) * | 2021-06-11 | 2022-12-13 | 四川大学 | A kind of preparation method of spherical CeO2 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113010A (en) * | 2007-07-04 | 2008-01-30 | 北京化工大学 | Microwave Assisted Preparation of Cerium Oxide Nanoparticles |
| CN102020306A (en) * | 2010-12-22 | 2011-04-20 | 江西师范大学 | Microwave rapid synthetic method of nanometer cerium oxide |
-
2012
- 2012-11-20 CN CN2012104732230A patent/CN102942204A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101113010A (en) * | 2007-07-04 | 2008-01-30 | 北京化工大学 | Microwave Assisted Preparation of Cerium Oxide Nanoparticles |
| CN102020306A (en) * | 2010-12-22 | 2011-04-20 | 江西师范大学 | Microwave rapid synthetic method of nanometer cerium oxide |
Non-Patent Citations (2)
| Title |
|---|
| 杨志杰: "氧化铈微纳结构材料的制备及性质研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
| 王孙昊: "一维CeO2纳米材料的微波合成与光催化性能研究", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI607969B (en) * | 2014-09-12 | 2017-12-11 | 台灣積體電路製造股份有限公司 | Method for manufacturing cerium dioxide powders and cerium dioxide powders |
| US11655405B2 (en) | 2014-09-12 | 2023-05-23 | Taiwan Semiconductor Manufacturing Company Limited | Method of manufacturing cerium dioxide powder and cerium dioxide powder |
| CN109438010A (en) * | 2018-11-29 | 2019-03-08 | 盛世生态环境股份有限公司 | A method of compost is prepared using garden waste and breeding wastewater |
| CN111579515A (en) * | 2020-05-26 | 2020-08-25 | 山东理工大学 | A method for oxidizing TMB with nano-cerium dioxide as simulated oxidase |
| CN115465879A (en) * | 2021-06-11 | 2022-12-13 | 四川大学 | A kind of preparation method of spherical CeO2 |
| CN115465879B (en) * | 2021-06-11 | 2023-06-02 | 四川大学 | Spherical CeO 2 Is prepared by the preparation method of (2) |
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Application publication date: 20130227 |