CN100586862C - Method for manufacturing high purity nano-cerium dioxide - Google Patents
Method for manufacturing high purity nano-cerium dioxide Download PDFInfo
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- CN100586862C CN100586862C CN200810034551A CN200810034551A CN100586862C CN 100586862 C CN100586862 C CN 100586862C CN 200810034551 A CN200810034551 A CN 200810034551A CN 200810034551 A CN200810034551 A CN 200810034551A CN 100586862 C CN100586862 C CN 100586862C
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- cerium dioxide
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Abstract
The invention relates to a preparation method of high purity nano-sized cerium dioxide, belonging to the technical field of inorganic material synthesis, which comprises the following steps: by Usingsoluble metal nitrate, N, and DMA as raw materials, hydrothermal reaction method is combined with solid phase reaction method, so as to synthesize cerium dioxide with the particle size distribution ofnanometer and stable chemical properties under different temperatures. The method of the invention has the advantages of strong operability, good reproducibility; moreover, the obtained product has the advantages of stable quality, even granules, and high purity.
Description
Technical field
The invention belongs to technical field of inorganic material synthesis, be specifically related to a kind of preparation method of high purity nano-cerium dioxide,
Background technology
Cerium dioxide is a kind of important rare earth material, all has a wide range of applications at aspects such as glass, pottery, abrasive material, catalyzer.Nano Ce O
2Be used widely in high-tech areas such as oxygen-sensitive material, Solid Oxide Fuel Cell, radioresistive glass, luminescent material and purifying vehicle exhausts because of having many-sided functional performance. nano Ce O
2Chemically machinery polished (CMP) slurry that can be used for integrated circuit (IC) chip processing is with nano Ce O
2Replace SiO
2As silicon chip and SiO
2The polishing particles of medium layer CMP process has that smooth quality is higher, polishing speed is faster, the better advantage of selectivity. so nano Ce O
2Be prepared into one of research focus in the Materials science.
At present, the normal preparation nano Ce O that adopts
2The method that has has solid phase method, the precipitator method, sol-gel method, hydrothermal method, high-temperature solid phase reaction method, spray pyrolysis, combustion method and microwave irradiation etc.Nano Ce O by these method preparations
2The uniform particles degree is not enough.By discovering (NO with Ce
3)
36H
2O and N, N N,N-DIMETHYLACETAMIDE (DMA) is a raw material, combines with solid reaction process by hydrothermal method and prepares nano ceric oxide.The products obtained therefrom steady quality, particle is more even, and the purity height.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of high purity nano-cerium dioxide
The preparation method of a kind of high purity nano-cerium dioxide that the present invention proposes, concrete steps are as follows:
(1) proportioning raw materials: with Ce (NO
3)
36H
2O and N, N N,N-DIMETHYLACETAMIDE (DMA) is a raw material, with Ce (NO
3)
36H
2O is configured to the solution that volumetric molar concentration is 0.1～0.4mol/l, according to Ce (NO
3)
36H
2O and N, the mol ratio of N N,N-DIMETHYLACETAMIDE (DMA) is two kinds of solution of mixed of 1: 5～1: 10, at room temperature stirs 0.5～1h, and it is fully reacted;
(2) hydrothermal synthesis reaction: the mixture of step (1) gained is placed the tetrafluoroethylene reactor, under 150～180 ℃ of temperature, react 24～72h; Cooling at room temperature obtains white suspension liquid then, filters, and gets white precipitate.
(3) filtration washing: filtration washing: pure water, absolute ethanol washing, to filter, drying obtains white powder;
(4) with the roasting of step (3) gained white powder, be cooled to room temperature then, promptly get desired product nano level CeO
2
Among the present invention, drying temperature is 60～80 ℃ described in the step (3), and be 18-30 hour time of drying.
Among the present invention, the described maturing temperature of step (4) is 400～800 ℃, and roasting time is 2-4 hour.
The present invention has prepared stable chemical performance, and size distribution is at nano level cerium dioxide particulate.Particle diameter is 30～60nm.This method is workable, favorable reproducibility, and products obtained therefrom steady quality, uniform particles, and purity height.
These purposes of the present invention, feature and advantage will become clearer after reading whole specification sheets in conjunction with the accompanying drawings.
Description of drawings
Fig. 1 is the embodiment of the invention 1 products therefrom CeO
2The X-ray diffraction spectrogram, can get CeO
2Be pure phase, calculate product particle diameter 30～60nm.
Fig. 2 is the embodiment of the invention 1 products therefrom CeO
2Transmission electron microscope picture, particle size with match by xrd figure result calculated.
Embodiment
Further specify the present invention below by embodiment, but protection scope of the present invention is not limited to these embodiment.
Embodiment 1
With Ce (NO
3)
36H
2O is the Ce (NO of 0.10mol/l for the preparation of raw material volumetric molar concentration
3)
3Solution.Measure N with graduated cylinder, N N,N-DIMETHYLACETAMIDE (DMA) is according to Ce (NO
3)
3With N, N N,N-DIMETHYLACETAMIDE (DMA) mol ratio is the above two kinds of solution of 1: 5 mixed, at room temperature stirs 1h, makes its thorough mixing.The mixture of gained is packed in the tetrafluoroethylene reactor, obtaining suspension liquid behind the reaction 24h under 160 ℃ of conditions, cooled and filtered obtains solid, with pure water and dehydrated alcohol repetitive scrubbing gained solid product, place drying under 70 ℃ of conditions of baking oven then, get white powder.The gained white powder 800 ℃ roasting temperature 2 hours, is cooled to room temperature, promptly obtains desired product.Result by xrd figure and transmission electron microscope can obtain product C eO
2Be pure phase, calculate product particle diameter 30～60nm.
With Ce (NO
3)
36H
2O is the Ce (NO of 0.40mol/l for the preparation of raw material volumetric molar concentration
3)
3Solution.Measure N with graduated cylinder, N N,N-DIMETHYLACETAMIDE (DMA) is according to Ce (NO
3)
3With N, N N,N-DIMETHYLACETAMIDE (DMA) mol ratio is the above two kinds of solution of 1: 10 mixed, at room temperature stirs 0.5h, makes its thorough mixing.The mixture of gained is packed in the tetrafluoroethylene reactor, obtaining suspension liquid behind the reaction 72h under 180 ℃ of conditions, cooled and filtered obtains solid, with pure water and dehydrated alcohol repetitive scrubbing gained solid product, place drying under 70 ℃ of conditions of baking oven then, get white powder.The gained white powder 400 ℃ roasting temperature 4 hours, is cooled to room temperature, promptly obtains desired product.Result by xrd figure and transmission electron microscope can obtain product C eO
2Be pure phase, calculate product particle diameter 30～60nm.
Embodiment 3
With Ce (NO
3)
36H
2O is the Ce (NO of 0.20mol/l for the preparation of raw material volumetric molar concentration
3)
3Solution.Measure N with graduated cylinder, N N,N-DIMETHYLACETAMIDE (DMA) is according to Ce (NO
3)
3With N, N N,N-DIMETHYLACETAMIDE (DMA) mol ratio is the above two kinds of solution of 1: 9 mixed, at room temperature stirs 0.5h, makes its thorough mixing.The mixture of gained is packed in the tetrafluoroethylene reactor, obtaining suspension liquid behind the reaction 48h under 150 ℃ of conditions, cooled and filtered obtains solid, with pure water and dehydrated alcohol repetitive scrubbing gained solid product, place drying under 70 ℃ of conditions of baking oven then, get white powder.The gained white powder 700 ℃ roasting temperature 2 hours, is cooled to room temperature, promptly obtains desired product.Result by xrd figure and transmission electron microscope can obtain product C eO
2Be pure phase, calculate product particle diameter 30～60nm.
Embodiment 4
With Ce (NO
3)
36H
2O is the Ce (NO of 0.30mol/l for the preparation of raw material volumetric molar concentration
3)
3Solution.Measure N with graduated cylinder, N N,N-DIMETHYLACETAMIDE (DMA) is according to Ce (NO
3)
3With N, N N,N-DIMETHYLACETAMIDE (DMA) mol ratio is the above two kinds of solution of 1: 8 mixed, at room temperature stirs 1h, makes its thorough mixing.The mixture of gained is packed in the tetrafluoroethylene reactor, obtaining suspension liquid behind the reaction 24h under 170 ℃ of conditions, cooled and filtered obtains solid, with pure water and dehydrated alcohol repetitive scrubbing gained solid product, place drying under 70 ℃ of conditions of baking oven then, get white powder.The gained white powder 500 ℃ roasting temperature 3 hours, is cooled to room temperature, promptly obtains desired product.Result by xrd figure and transmission electron microscope can obtain product C eO
2Be pure phase, calculate product particle diameter 30～60nm.
Embodiment 5
With Ce (NO
3)
36H
2O is the Ce (NO of 0.10mol/l for the preparation of raw material volumetric molar concentration
3)
3Solution.Measure N with graduated cylinder, N N,N-DIMETHYLACETAMIDE (DMA) is according to Ce (NO
3)
3With N, N N,N-DIMETHYLACETAMIDE (DMA) mol ratio is the above two kinds of solution of 1: 7 mixed, at room temperature stirs 0.7h, makes its thorough mixing.The mixture of gained is packed in the tetrafluoroethylene reactor, obtaining suspension liquid behind the reaction 48h under 160 ℃ of conditions, cooled and filtered obtains solid, with pure water and dehydrated alcohol repetitive scrubbing gained solid product, place drying under 70 ℃ of conditions of baking oven then, get white powder.The gained white powder 600 ℃ roasting temperature 2 hours, is cooled to room temperature, promptly obtains desired product.Result by xrd figure and transmission electron microscope can obtain product C eO
2Be pure phase, calculate product particle diameter 30～60nm.
Embodiment 6
With Ce (NO
3)
36H
2O is the Ce (NO of 0.40mol/l for the preparation of raw material volumetric molar concentration
3)
3Solution.Measure N with graduated cylinder, N N,N-DIMETHYLACETAMIDE (DMA) is according to Ce (NO
3)
3With N, N N,N-DIMETHYLACETAMIDE (DMA) mol ratio is the above two kinds of solution of 1: 6 mixed, at room temperature stirs 0.5h, makes its thorough mixing.The mixture of gained is packed in the tetrafluoroethylene reactor, obtaining suspension liquid behind the reaction 48h under 160 ℃ of conditions, cooled and filtered obtains solid, with pure water and dehydrated alcohol repetitive scrubbing gained solid product, place drying under 70 ℃ of conditions of baking oven then, get white powder.The gained white powder 700 ℃ roasting temperature 2 hours, is cooled to room temperature, promptly obtains desired product.Result by xrd figure and transmission electron microscope can obtain product C eO
2Be pure phase, calculate product particle diameter 30～60nm.
Claims (3)
1, a kind of preparation method of high purity nano-cerium dioxide is characterized in that concrete steps are as follows:
(1) proportioning raw materials: with Ce (NO
3)
36H
2O and N, N N,N-DIMETHYLACETAMIDE are raw material, with Ce (NO
3)
36H
2O is configured to the solution that volumetric molar concentration is 0.1～0.4mol/l, according to Ce (NO
3)
36H
2O and N, the mol ratio of N N,N-DIMETHYLACETAMIDE is two kinds of solution of mixed of 1: 5～1: 10, at room temperature stirs 0.5～1h, and it is fully reacted;
(2) hydrothermal synthesis reaction: the mixture of step (1) gained is placed the tetrafluoroethylene reactor, under 150～180 ℃ of temperature, react 24～72h; Cooling at room temperature obtains white suspension liquid then, filters, and gets white precipitate;
(3) filtration washing: pure water and absolute ethanol washing, to filter, drying obtains white powder;
(4) with the roasting of step (3) gained white powder, be cooled to room temperature then, promptly get desired product nano level CeO
2
2, the preparation method of high purity nano-cerium dioxide according to claim 1 is characterized in that drying temperature is 60-80 ℃ described in the step (3), and be 18-30 hour time of drying.
3, the preparation method of high purity nano-cerium dioxide according to claim 1 is characterized in that the described maturing temperature of step (4) is 400～800 ℃, and roasting time is 2-4 hour.
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| CN100586862C true CN100586862C (en) | 2010-02-03 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101825551B (en) * | 2009-07-23 | 2011-07-27 | 中国科学院过程工程研究所 | Cerium dioxide microsphere used as dimension standard material |
| CN101875502A (en) * | 2010-07-07 | 2010-11-03 | 淄博广通化工有限责任公司 | Hard aggregation-free high-purity nanometer cerium oxide powder material and preparation method thereof |
| CN102275971A (en) * | 2011-05-26 | 2011-12-14 | 哈尔滨工业大学 | Method for preparing nano-sized cerium dioxide through room temperature solid phase reaction |
| CN103086417A (en) * | 2013-01-25 | 2013-05-08 | 吴江创源新材料科技有限公司 | Shape controlled cerium oxide particle, as well as preparation method and application thereof |
| CN105585043B (en) * | 2016-03-11 | 2017-04-12 | 九江学院 | Preparation method of flowerlike cerium oxide nano-material |
| CN106745166A (en) * | 2016-11-24 | 2017-05-31 | 郑州轻工业学院 | A kind of synthetic method of quantum dot cerium oxide/modified oxidized cerium nano material |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1840480A (en) * | 2005-03-29 | 2006-10-04 | 中国科学院大连化学物理研究所 | Cerium oxide nano materials and its preparation and use |
| CN101104524A (en) * | 2006-07-14 | 2008-01-16 | 中南大学 | Process for preparing nanometer cerium dioxide |
| CN101117233A (en) * | 2007-07-23 | 2008-02-06 | 北京科技大学 | Method for preparing high specific surface area meso-porous cerium dioxide micro-balloon |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1840480A (en) * | 2005-03-29 | 2006-10-04 | 中国科学院大连化学物理研究所 | Cerium oxide nano materials and its preparation and use |
| CN101104524A (en) * | 2006-07-14 | 2008-01-16 | 中南大学 | Process for preparing nanometer cerium dioxide |
| CN101117233A (en) * | 2007-07-23 | 2008-02-06 | 北京科技大学 | Method for preparing high specific surface area meso-porous cerium dioxide micro-balloon |
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