CN101113010A - Method for preparing cerium oxide nano particle by auxiliary microwave - Google Patents
Method for preparing cerium oxide nano particle by auxiliary microwave Download PDFInfo
- Publication number
- CN101113010A CN101113010A CNA2007101182685A CN200710118268A CN101113010A CN 101113010 A CN101113010 A CN 101113010A CN A2007101182685 A CNA2007101182685 A CN A2007101182685A CN 200710118268 A CN200710118268 A CN 200710118268A CN 101113010 A CN101113010 A CN 101113010A
- Authority
- CN
- China
- Prior art keywords
- microwave
- solution
- cerium
- alkali lye
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
A method to microwave-assisted prepare ceria Nano particles pertains to the preparation technology field of the ceria Nano particles. First cerium ion solution and alkali liquor are mixed and then the mixture is put into a microwave high pressure reaction cylinder, at last the ceria Nano particles, chemical formula of which is CeO2, are obtained by microwave-assisted reaction. The invention has the advantages of simple preparation process, short reaction time, and energy conservation, small particle diameter of ceria Nano particles, good dispersion and structured appearance.
Description
Technical field
The invention belongs to the preparing technical field of cerium oxide nano particle, a kind of method of preparing cerium oxide nano particle by auxiliary microwave particularly is provided.
Background technology
Nano Ce O
2Be the extremely wide Industrial materials of a kind of cheapness and purposes, it can be used as the main body material of the oxygen ion conductor of Solid Oxide Fuel Cell (SOFC), can be used as the rumbling compound and the glass decolouring finings of luminescent material, electronic ceramics, glass, can be used as the three-element catalytic auxiliary agent at the purifying vehicle exhaust face, it also is the important composition composition of superconductor, pottery, petroleum cracking catalyzer and homogeneous catalyst, thereby the exploration of the new technology of preparing of cerium oxide nano particle has become hot research problem in recent years.Hydrothermal method is a kind of chemical process for preparing nano material, this method provides physics that can't obtain and chemical environment for the reaction and the crystallization of various precursors under condition of normal pressure, because not needing high temperature sintering in the preparation process handles, avoid the powder hard aggregation that may form, the powder purity height that makes, good dispersity, and pollute little, therefore, be subjected to people's extensive attention in recent years.In traditional hydrothermal method, adopt the common heating mode, for example: at Mater Chem andPhys, 2000, among the 64:229-240, the nitrate of human Ce (III) such as J.H Chem Lin, vitriol and the ammonium sulfate of Ce (IV) have prepared CeO at 180 ℃
2Nanoparticle.But this method long reaction time heats inhomogeneously, and heat-up rate is slow, and the particle crystalline form that obtains is not very regular.In view of the problem that exists in the above-mentioned preparation process, preparation is simple in exploration, less energy consumption, and preparation crystalline form, granularity and the good cerium oxide nano particle method of distribution are very necessary.
Summary of the invention
The object of the present invention is to provide a kind of method of preparing cerium oxide nano particle by auxiliary microwave, solved with traditional Hydrothermal Preparation cerium oxide nano particle long reaction time, energy consumption height, problems such as particle crystalline form irregularity.
Technical scheme of the present invention is at first cerium ion solution to be mixed with alkali lye, puts into the microwave high pressure retort then, obtains cerium oxide nano particle through the microwave-assisted reaction, and its chemical formula is CeO
2, its processing step is as follows:
1, preparation feedback mixed solution
The preparation cerium solution of 0.1-1mol/L and the alkali lye of 0.1-1mol/L concentration are got the cerium solution that 2mL-20mL prepares and are put into beaker, add template, stir, and the alkali lye that drips 2mL-20mL again mixes and stirs, and prepares reaction mixture;
2, microwave-assisted reaction
The reaction mixture of step 1 preparation is put into the microwave high pressure retort, under 80-200 ℃, carry out high-temperature high-voltage reaction 2min-10h with microwave-assisted, adopt the stove internal cooling afterwards, obtain containing product C eO to room temperature with the power of 200W-1000W
2Solution;
3, aftertreatment
The solution of step 2 preparation is taken out, use deionized water, absolute ethanol washing product 1-5 time respectively, centrifugation 40-80 ℃ of following 6h-24h drying, is ground, and obtains particle diameter at nano level, good dispersity, the regular cube fluorite structure CeO of pattern
2Powder.
Cerium solution of the present invention is Ce (NO
3)
3, Ce (Ac)
3, Ce (SO
4)
2In any; Described alkali lye is NaOH, NaAc, (NH
2)
2CO, NH
3H
2The mixture of any or its any 2-3 kind among the O; Described template is the mixture of any or its any 2-3 kind among SDS, CTAB, PEG, TEA, the TX-100.
Compared with prior art, the invention has the advantages that:
Because adopt microwave heating, rate of heating is fast, shortened the time of reaction, reduced energy consumption; In addition, advantage such as microwave heating has from inside to outside, selectivity is good, homogeneous heating, heat-up rate are fast, therefore prepared product has better crystalline form, granularity and distribution; Present method preparation technology is simple, easy control of reaction conditions, the product purity height.
Description of drawings
Fig. 1 prepares the preparation flow synoptic diagram of nano-cerium oxide for microwave-assisted of the present invention.
Fig. 2 is product C eO in the embodiment of the invention 1
2The XRD spectra of powder.
Fig. 3 is product C eO in the embodiment of the invention 1
2The TEM of powder (100K) photograph.
Fig. 4 is product C eO in the embodiment of the invention 1
2The TEM of powder (200K) photograph
Embodiment
Embodiment 1
Ce (the NO of preparation 0.1mol/L
3)
3The NaAc solution of solution and 0.4mol/L is got the 0.1mol/LCe (NO of 10ml
3)
3Solution is put into beaker, adds 2.73gCTAB and stirs, and adds the 0.4mol/L NaAc solution of 10ml again, mixes and stirs.Afterwards mixed solution is put into the microwave high pressure reactor and reacted, react 6h down at 180 ℃, the stove internal cooling is to room temperature.Take out reacted solution, use deionized water, absolute ethanol washing 3 times respectively, centrifugation, drying is ground, and obtains cerium oxide nano-powder.
The gained powder is carried out the X-ray diffraction analysis, the result as shown in Figure 2, the diffraction peak that occurs among the figure is CeO
2Characteristic diffraction peak, confirm that the product obtain is CeO
2, and no any impurity in the product.
The TEM transmission electron microscope photo of product as shown in Figure 3, Figure 4, as can be seen from the figure, the CeO that this method makes
2Be nanoparticle, particle diameter is at 10-20nm, and crystalline form is a cube fluorite structure, and good dispersity, pattern are regular.
Embodiment 2
With Ce (Ac)
3And H
2O is a reactant, adopts condition and the method identical with embodiment 1, can prepare particle diameter equally at nano level, uniform CeO
2Powder.
Embodiment 3
With Ce (NO
3)
3With NaOH be reactant, adopt condition and the method identical with embodiment 1, can prepare particle diameter equally at nano level, uniform CeO
2Powder.
Claims (5)
1. the method for a preparing cerium oxide nano particle by auxiliary microwave is at first mixed cerium ion solution with alkali lye, puts into the microwave high pressure retort then, obtains cerium oxide nano particle through the microwave-assisted reaction, and its chemical formula is CeO
2, its processing step is:
(1) preparation feedback mixed solution
The preparation cerium solution of 0.1-1mol/L and the alkali lye of 0.1-1mol/L concentration are got the cerium solution that 2mL-20mL prepares and are put into beaker, add template, stir, and the alkali lye that drips 2mL-20mL again mixes and stirs, and prepares reaction mixture;
(2) microwave-assisted reaction
The reaction mixture of step (1) preparation is put into the microwave high pressure retort, under 80-200 ℃, carry out high-temperature high-voltage reaction 2min-10h with microwave-assisted, adopt the stove internal cooling afterwards, obtain containing product C eO to room temperature with the power of 200W-1000W
2Solution;
(3) aftertreatment
The solution of step (2) preparation is taken out, use deionized water, absolute ethanol washing product 1-5 time respectively, centrifugation, at 40-80 ℃ of dry 6h-24h down, grinding obtains particle diameter at nano level, the CeO of cube fluorite structure that good dispersity, pattern are regular
2Powder.
2. method according to claim 1 is characterized in that: described cerium solution is Ce (NO
3)
3, Ce (Ac)
3, Ce (SO
4)
2In any.
3. method according to claim 1 is characterized in that: described alkali lye is NaOH, NaAc, (NH
2)
2CO, NH
3H
2The mixture of any or its any 2-3 kind among the O.
4. method according to claim 1 is characterized in that: described template is the mixture of any or its any 2-3 kind among SDS, CTAB, PEG, TEA, the TX-100.
5. method according to claim 1 is characterized in that: cerium solution, alkali lye, template blending ratio are 1: 1: 1-1: 80: 10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101182685A CN101113010A (en) | 2007-07-04 | 2007-07-04 | Method for preparing cerium oxide nano particle by auxiliary microwave |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101182685A CN101113010A (en) | 2007-07-04 | 2007-07-04 | Method for preparing cerium oxide nano particle by auxiliary microwave |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101113010A true CN101113010A (en) | 2008-01-30 |
Family
ID=39021568
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101182685A Pending CN101113010A (en) | 2007-07-04 | 2007-07-04 | Method for preparing cerium oxide nano particle by auxiliary microwave |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101113010A (en) |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020306A (en) * | 2010-12-22 | 2011-04-20 | 江西师范大学 | Microwave rapid synthetic method of nanometer cerium oxide |
| CN102942204A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Method for preparing cerium dioxide nanometer powder |
| CN102942206A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Method for preparing cerium dioxide nanometer hollow spheres |
| CN102951940A (en) * | 2012-11-05 | 2013-03-06 | 昆明理工大学 | Mesoporous cerium dioxide material preparation method |
| CN103011235A (en) * | 2012-11-28 | 2013-04-03 | 江西师范大学 | Industrial microwave rapid synthesis method of ultra-large specific surface area nano cerium dioxide |
| RU2487753C2 (en) * | 2008-12-17 | 2013-07-20 | Серион Текнолоджи, Инк. | Fuel additive containing cerium dioxide nanoparticles with altered structure |
| US9221032B2 (en) | 2006-09-05 | 2015-12-29 | Cerion, Llc | Process for making cerium dioxide nanoparticles |
| US9303223B2 (en) | 2006-09-05 | 2016-04-05 | Cerion, Llc | Method of making cerium oxide nanoparticles |
| CN109399689A (en) * | 2018-12-17 | 2019-03-01 | 中铝广西国盛稀土开发有限公司 | A method of rare earth oxide is prepared using microwave technology |
| US10435639B2 (en) | 2006-09-05 | 2019-10-08 | Cerion, Llc | Fuel additive containing lattice engineered cerium dioxide nanoparticles |
| US10500228B1 (en) * | 2016-04-26 | 2019-12-10 | Battelle Memorial Institute | Nanoparticles, methods for producing nanoparticles and nanoparticle generators |
| CN112266730A (en) * | 2020-12-04 | 2021-01-26 | 内蒙古科技大学 | Preparation method of fluorinated cerium dioxide polishing powder under microwave condition |
| CN112340766A (en) * | 2020-11-27 | 2021-02-09 | 重庆大学 | Cerium oxide modified microwave hydrothermal carbon and preparation method and application thereof |
-
2007
- 2007-07-04 CN CNA2007101182685A patent/CN101113010A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10435639B2 (en) | 2006-09-05 | 2019-10-08 | Cerion, Llc | Fuel additive containing lattice engineered cerium dioxide nanoparticles |
| US9221032B2 (en) | 2006-09-05 | 2015-12-29 | Cerion, Llc | Process for making cerium dioxide nanoparticles |
| US9303223B2 (en) | 2006-09-05 | 2016-04-05 | Cerion, Llc | Method of making cerium oxide nanoparticles |
| US9340738B2 (en) | 2006-09-05 | 2016-05-17 | Cerion, Llc | Method of making cerium oxide nanoparticles |
| US9993803B2 (en) | 2006-09-05 | 2018-06-12 | Cerion, Llc | Method of preparing cerium dioxide nanoparticles |
| RU2487753C2 (en) * | 2008-12-17 | 2013-07-20 | Серион Текнолоджи, Инк. | Fuel additive containing cerium dioxide nanoparticles with altered structure |
| CN102020306A (en) * | 2010-12-22 | 2011-04-20 | 江西师范大学 | Microwave rapid synthetic method of nanometer cerium oxide |
| CN102951940A (en) * | 2012-11-05 | 2013-03-06 | 昆明理工大学 | Mesoporous cerium dioxide material preparation method |
| CN102942204A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Method for preparing cerium dioxide nanometer powder |
| CN102942206A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Method for preparing cerium dioxide nanometer hollow spheres |
| CN103011235A (en) * | 2012-11-28 | 2013-04-03 | 江西师范大学 | Industrial microwave rapid synthesis method of ultra-large specific surface area nano cerium dioxide |
| US10500228B1 (en) * | 2016-04-26 | 2019-12-10 | Battelle Memorial Institute | Nanoparticles, methods for producing nanoparticles and nanoparticle generators |
| CN109399689A (en) * | 2018-12-17 | 2019-03-01 | 中铝广西国盛稀土开发有限公司 | A method of rare earth oxide is prepared using microwave technology |
| CN112340766A (en) * | 2020-11-27 | 2021-02-09 | 重庆大学 | Cerium oxide modified microwave hydrothermal carbon and preparation method and application thereof |
| CN112340766B (en) * | 2020-11-27 | 2022-02-01 | 重庆大学 | Cerium oxide modified microwave hydrothermal carbon and preparation method and application thereof |
| CN112266730A (en) * | 2020-12-04 | 2021-01-26 | 内蒙古科技大学 | Preparation method of fluorinated cerium dioxide polishing powder under microwave condition |
| CN112266730B (en) * | 2020-12-04 | 2021-08-31 | 内蒙古科技大学 | Preparation method of fluorinated cerium dioxide polishing powder under microwave condition |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101113010A (en) | Method for preparing cerium oxide nano particle by auxiliary microwave | |
| Mi et al. | Synthesis of BaTiO3 nanoparticles by sol-gel assisted solid phase method and its formation mechanism and photocatalytic activity | |
| CN103449496A (en) | Nano cerium oxide and preparation method thereof | |
| CN111908922A (en) | Low-temperature synthesized rare earth hafnate high-entropy ceramic powder and preparation method thereof | |
| CN105129805B (en) | Preparation method of silicon oxide/tin antimony oxide/zinc oxide ternary composite material | |
| CN103157461A (en) | Nanometer photocatalyst bismuth tungstate and preparation method thereof | |
| CN103240073B (en) | Zn<2+>-doped BiVO4 visible-light-driven photocatalyst and preparation method thereof | |
| CN102126752B (en) | Method for preparing tetragonal phase zirconia nanorod | |
| CN105170173A (en) | Perovskite material/organic polymer compound photocatalyst, preparation and application | |
| CN105271405A (en) | Material based on bismuth oxycarbonate or bismuth oxide nano tube and preparation method thereof | |
| CN112058270A (en) | Flaky La0.8Sr0.2CoO3In-situ synthesis method and application of perovskite catalyst | |
| CN109569607A (en) | A kind of preparation method of novel cobalt-based composite material | |
| Chen et al. | Synthesis of and densification of oxygen-conducting La0. 8Sr0. 2Ga0. 8Mg0. 2O2. 8 nano powder prepared from a low temperature hydrothermal urea precipitation process | |
| CN107857300B (en) | A kind of preparation method of β type bismuth oxide | |
| Yang et al. | Facile microwave-assisted synthesis and effective photocatalytic hydrogen generation of Zn 2 GeO 4 with different morphology | |
| CN102070178A (en) | Method for preparing yttrium oxide micro-nano-materials based on hydrothermal technology regulation and control | |
| CN108722486A (en) | A kind of preparation method of narrowband carbonitride modification ferrous metals organic backbone composite photo-catalyst | |
| Mao et al. | Template-free synthesis of VO x hierarchical hollow spheres | |
| CN107473737B (en) | Composite zirconia powder for solid oxide fuel cell and preparation method thereof | |
| CN103113955A (en) | Preparation method of nano porous iron-base oxygen carrier for biological oil chemical-looping hydrogen production | |
| CN103553032B (en) | Method for preparing reduced graphene oxide/cerium oxide nano-bulk composite | |
| CN106186036B (en) | A kind of preparation method of hexagon cerium dioxide nano sheet material | |
| CN112408320A (en) | Load type double-active metal composite oxygen carrier and preparation method and application thereof | |
| CN102380408A (en) | Method for preparing nanometer sodium metatantalate photocatalysts | |
| CN102502768B (en) | Method for preparing special-shaped lanthanum cuprate (La2CuO4) powder bodies by sol-gel method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Open date: 20080130 |