CN104310455A - Preparation method of cerium oxide nanosheet - Google Patents
Preparation method of cerium oxide nanosheet Download PDFInfo
- Publication number
- CN104310455A CN104310455A CN201410529975.3A CN201410529975A CN104310455A CN 104310455 A CN104310455 A CN 104310455A CN 201410529975 A CN201410529975 A CN 201410529975A CN 104310455 A CN104310455 A CN 104310455A
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- CN
- China
- Prior art keywords
- cerium oxide
- preparation
- cerium
- oxide nanosheet
- oxide nano
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/36—Spheres fragmented
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention relates to a preparation method of a cerium oxide nanosheet which is prepared by using a direct precipitation method by using cerium acetate hydrate powder as a raw material, ammonium hydrogen carbonate as a precipitator and water as a solvent, wherein the cerium oxide nanosheet is 25-30nm thick. The preparation method comprises the following steps: adding the cerium acetate hydrate powder into a 0.03-0.05mol/L ammonium hydrogen carbonate aqueous solution and continuously magnetically stirring to react for 60 minutes at room temperature; carrying out centrifugal separation on a reaction product and washing a filter cake by absolute ethyl alcohol and then carrying out centrifugal separation again, and naturally drying the filter cake at room temperature; and then, annealing the dried product at 600 DEG C in a muffle furnace for 60 minutes to obtain the cerium oxide nanosheet, wherein the mass ratio of cerium acetate hydrate and ammonium hydrogen carbonate is (1-1.3): 1. The preparation method provided by the invention is simple in process, short in production period, low in cost and suitable for scaled production. The cerium oxide nanosheet can be used in the fields of automobile emission purification, catalysts, mechanical polishing and the like.
Description
Technical field
The present invention relates to a kind of preparation method of cerium oxide nano-plate, belong to technical field of inorganic nanometer material.
Background technology
Cerium oxide CeO
2be a kind of very important rare earth oxide, it has wide application development prospect in fields such as purifying vehicle exhaust, catalyzer, mechanical polishing, optical materials.Two-dimensional sheet nano material is owing to having larger specific surface area, these bill of material are made to reveal special surface tissue and characteristic electron, there is excellent electricity and mechanical property, particularly in the photoelectrochemistry field depending on material surface characteristic, there is important potential application.Therefore the controlledly synthesis research of two-dimensional sheet cerium oxide nano materials just causes the great interest of numerous scientific workers, and has done a large amount of research work.But cerium oxide is not lamellar structure compound, the nano-cerium oxide generally prepared is spherical, bar-shaped, the shape such as polyhedron or flowers, and its crystal face such as highly active (100), (001) cannot fully expose, and reduces its performance.Therefore, by innovation and the improvement of nano material technology, obtain platy cerium oxide nano material, reduce the thickness of cerium oxide nano-plate, increasing specific surface area, raising dispersiveness, more high reactivity crystal face is come out, improve it and store up/put oxygen ability and catalytic oxidation activity, then become a Some Questions To Be Researched of modern materials science and chemistry.
At present, CeO
2the preparation method of nanometer sheet material mainly contains the precipitator method, water (solvent) hot method, sol-gel method, combustion method, thermal decomposition method etc.Adopt these methods, people have successfully obtained the CeO of many different-shapes
2nano material, also comprises sheet structure CeO
2nano material.As cerous nitrate salt to be placed in the solvent that there is tensio-active agent and precipitation agent by (patent of invention CN 101264922 B) such as Zhang Dengsong, reflux, centrifugal drying calcines to obtain CeO
2rhombus nanometer sheet; Dong Xiangting etc. (patent of invention CN101792170A) CeO that adopted electrostatic spinning technique to prepare
2nano belt, wide 3-5 μm, thick 65-120 nm; Zhang Dengsong etc. (patent of invention CN101407331A) adopt and cerium salt and cetyl trimethylammonium bromide are dissolved in deionized water, then obtain CeO 100-180 DEG C of hydro-thermal reaction
2nanometer sheet; Wang Dianyuan etc. (Angew Chem Int Ed, 2011,50,4378-4381) adopt thermolysis cerous acetate in oleic acid, oleyl amine, octadecylene solvent, obtain the CeO that 2 nm are thick
2nanometer sheet.All in all, aforesaid method is prepared platy cerium oxide nano material and is all needed tensio-active agent, or comparatively high temps (as hydrothermal method), production technique more complicated, and cost is higher, and the cycle is long, is unfavorable for extensive preparation and suitability for industrialized production.
Compared with above-mentioned synthetic method, Direct precipitation rule is more easy, with short production cycle, and temperature of reaction is low, with low cost, and efficiency is high, is more suitable for the large-scale production of two dimensional oxidation cerium nanometer sheet material.
Summary of the invention
The present invention be directed to the deficiency of existing two dimensional oxidation cerium nanometer sheet material synthesis technology, propose the preparation method of a kind of simple process, cerium oxide nano-plate with low cost.The method can solve the problem that cerium oxide nano-plate thickness is large, bad dispersibility, high reactivity crystal face can not fully expose, thus improves it and store up/put oxygen ability and catalytic oxidation activity, and then improves its application performance in the field such as vehicle exhaust, catalyzer.
The preparation method of a kind of cerium oxide nano-plate of the present invention is specific as follows:
With hydrate cerium acetate powder for raw material, bicarbonate of ammonia is precipitation agent, and water is solvent, prepares cerium oxide nano sheet material by direct precipitation method, join in the ammonium bicarbonate aqueous solution of 0.03 ~ 0.05 mol/L by hydrate cerium acetate powder, room temperature with constant magnetic agitation reacts 60 min; By reaction product centrifugation, recentrifuge process after filter cake absolute ethanol washing, by filter cake seasoning at ambient temperature; Then anneal desciccate in 600 DEG C of retort furnaces 60 min, obtains cerium oxide nano sheet material; Wherein the mass ratio of hydrate cerium acetate, bicarbonate of ammonia is 1 ~ 1.3:1.
Described hydrate cerium acetate, the mass ratio of bicarbonate of ammonia are preferably 1.3:1.
beneficial effect of the present invention is:
(1) bicarbonate of ammonia of the present invention water-soluble after, there is two hydrolysis, produce OH
-, CO
3 2-ion, the aqueous solution is weakly alkaline; In addition, hydrate cerium acetate dissolves slowly in ammonium bicarbonate soln, dissolves, while the Ce ionized out
3+oH in ion and solution
-, CO
3 2-in conjunction with generation CeOHCO
3﹒ nH
2o nano level nucleus.CeOHCO
3﹒ nH
2o is a kind of lamellar compound, CeOHCO in reaction process
3﹒ nH
2o nucleus is constantly grown up, and anisotropic growth, the final sheet CeOHCO formed
3﹒ nH
2o nano material is annealed through retort furnace, can obtain sheet CeO
2nano material, nanometer sheet thickness 25 ~ 30 nm, specific surface area is large, good dispersity.
(2) synthesis technique of the present invention is easy, and reaction time is short, with low cost, is applicable to large-scale production.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope TEM photo of cerium oxide nano-plate.
Embodiment
embodiment 1:
Take bicarbonate of ammonia (NH
4hCO
3) 0.079g is in 50ml beaker, add 20ml deionized water, stirring at room temperature, to dissolving completely, obtains ammonium bicarbonate aqueous solution; Weigh hydrate cerium acetate (Ce (Ac)
3﹒ nH
2o) powder 0.1g, in the above-mentioned solution of direct disposable input, room temperature lower magnetic force stirs 60 minutes.To react final gained mixture centrifugal throw out, then use deionized water repetitive scrubbing, dry.Again by product in retort furnace 600 DEG C annealing 1 hour, obtain cerium oxide nano-plate.
embodiment 2:
Take bicarbonate of ammonia (NH
4hCO
3) 0.079g is in 50ml beaker, add 33ml deionized water, stirring at room temperature, to dissolving completely, obtains ammonium bicarbonate aqueous solution; Weigh hydrate cerium acetate (Ce (Ac)
3﹒ nH
2o) powder 0.079g, in the above-mentioned solution of direct disposable input, room temperature lower magnetic force stirs 60 minutes.To react final gained mixture centrifugal throw out, then use deionized water repetitive scrubbing, dry.Again by product in retort furnace 600 DEG C annealing 1 hour, obtain cerium oxide nano-plate.
Claims (2)
1. the preparation method of a cerium oxide nano-plate, it is characterized in that: with hydrate cerium acetate powder for raw material, bicarbonate of ammonia is precipitation agent, water is solvent, cerium oxide nano sheet material is prepared by direct precipitation method, join in the ammonium bicarbonate aqueous solution of 0.03 ~ 0.05 mol/L by hydrate cerium acetate powder, room temperature with constant magnetic agitation reacts 60 min; By reaction product centrifugation, recentrifuge process after filter cake absolute ethanol washing, by filter cake seasoning at ambient temperature; Then anneal desciccate in 600 DEG C of retort furnaces 60 min, obtains cerium oxide nano sheet material; Wherein the mass ratio of hydrate cerium acetate, bicarbonate of ammonia is 1 ~ 1.3:1.
2. a preparation method for cerium oxide nano-plate, is characterized in that: described hydrate cerium acetate, the mass ratio of bicarbonate of ammonia are preferably 1.3:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410529975.3A CN104310455A (en) | 2014-10-10 | 2014-10-10 | Preparation method of cerium oxide nanosheet |
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|---|---|---|---|
| CN201410529975.3A CN104310455A (en) | 2014-10-10 | 2014-10-10 | Preparation method of cerium oxide nanosheet |
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| Publication Number | Publication Date |
|---|---|
| CN104310455A true CN104310455A (en) | 2015-01-28 |
Family
ID=52365809
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| CN201410529975.3A Pending CN104310455A (en) | 2014-10-10 | 2014-10-10 | Preparation method of cerium oxide nanosheet |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106186036A (en) * | 2016-07-10 | 2016-12-07 | 九江学院 | A kind of preparation method of hexagon cerium dioxide nano sheet material |
| CN107446341A (en) * | 2017-08-23 | 2017-12-08 | 华南理工大学 | A kind of fire-retardant, less toxic TPUE/cerium oxide nano-plate nano composite material and preparation method thereof |
| CN111715208A (en) * | 2020-04-07 | 2020-09-29 | 盐城师范学院 | CeO (CeO)2Preparation method of composite photocatalytic material and application of composite photocatalytic material in photocatalytic hydrogen production |
| CN112704736A (en) * | 2021-01-08 | 2021-04-27 | 深圳万物创新集团有限公司 | CeO (CeO)2/MXene composite two-dimensional material and preparation method and application thereof |
| CN113548686A (en) * | 2021-06-04 | 2021-10-26 | 江汉大学 | Cerium dioxide nano material and preparation method and application thereof |
Citations (4)
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| CN1683248A (en) * | 2004-04-14 | 2005-10-19 | 北京方正稀土科技研究所有限公司 | Process for preparing nano cerium dioxide |
| US20070107318A1 (en) * | 2005-11-14 | 2007-05-17 | Oh Myoung H | Cerium carbonate powder, cerium oxide powder, method for preparing the same, and CMP slurry comprising the same |
| US20110281112A1 (en) * | 2010-05-13 | 2011-11-17 | Han Kwon Chang | Method for producing cerium dioxide nanopowder by flame spray pyrolysis and cerium dioxide nanopowder produced by the method |
| CN103991891A (en) * | 2014-05-08 | 2014-08-20 | 华东理工大学 | Preparation method of flaky nano-cerium oxide |
-
2014
- 2014-10-10 CN CN201410529975.3A patent/CN104310455A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1683248A (en) * | 2004-04-14 | 2005-10-19 | 北京方正稀土科技研究所有限公司 | Process for preparing nano cerium dioxide |
| US20070107318A1 (en) * | 2005-11-14 | 2007-05-17 | Oh Myoung H | Cerium carbonate powder, cerium oxide powder, method for preparing the same, and CMP slurry comprising the same |
| US20110281112A1 (en) * | 2010-05-13 | 2011-11-17 | Han Kwon Chang | Method for producing cerium dioxide nanopowder by flame spray pyrolysis and cerium dioxide nanopowder produced by the method |
| CN103991891A (en) * | 2014-05-08 | 2014-08-20 | 华东理工大学 | Preparation method of flaky nano-cerium oxide |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106186036A (en) * | 2016-07-10 | 2016-12-07 | 九江学院 | A kind of preparation method of hexagon cerium dioxide nano sheet material |
| CN106186036B (en) * | 2016-07-10 | 2017-10-24 | 九江学院 | A kind of preparation method of hexagon cerium dioxide nano sheet material |
| CN107446341A (en) * | 2017-08-23 | 2017-12-08 | 华南理工大学 | A kind of fire-retardant, less toxic TPUE/cerium oxide nano-plate nano composite material and preparation method thereof |
| CN107446341B (en) * | 2017-08-23 | 2020-09-22 | 华南理工大学 | Flame-retardant low-toxicity thermoplastic polyurethane elastomer/cerium oxide nanosheet nanocomposite and preparation method thereof |
| CN111715208A (en) * | 2020-04-07 | 2020-09-29 | 盐城师范学院 | CeO (CeO)2Preparation method of composite photocatalytic material and application of composite photocatalytic material in photocatalytic hydrogen production |
| CN112704736A (en) * | 2021-01-08 | 2021-04-27 | 深圳万物创新集团有限公司 | CeO (CeO)2/MXene composite two-dimensional material and preparation method and application thereof |
| CN113548686A (en) * | 2021-06-04 | 2021-10-26 | 江汉大学 | Cerium dioxide nano material and preparation method and application thereof |
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Application publication date: 20150128 |