CN109678193A - A kind of preparation method of ceria nanoparticles - Google Patents
A kind of preparation method of ceria nanoparticles Download PDFInfo
- Publication number
- CN109678193A CN109678193A CN201811587542.8A CN201811587542A CN109678193A CN 109678193 A CN109678193 A CN 109678193A CN 201811587542 A CN201811587542 A CN 201811587542A CN 109678193 A CN109678193 A CN 109678193A
- Authority
- CN
- China
- Prior art keywords
- preparation
- colloidal sol
- ceria nanoparticles
- temperature
- nanoparticles according
- 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.)
- Granted
Links
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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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 present invention relates to a kind of preparation methods of ceria nanoparticles, belong to nano-powder material field, method includes the following steps: (1) configures cerous nitrate-complexing agent aqueous solution, and adjust pH, and stirring forms colloidal sol;(2) stable reverse micro emulsion is formed in the mixed liquor of surfactant, cosurfactant and hexamethylene using colloidal sol as Aqueous dispersions, gel particle is made by reacting;(3) gel particle freezes, filters, drying, calcining and to obtain ceria nanoparticles by cooling.Nano-cerium oxide partial size prepared by the present invention is small controllably, pattern is uniform, reunion is lower, high surface activity.Solve the problems, such as that hard aggregation occurs for conventional sol-gel processes micelle in drying and heat treatment, and preparation process of the present invention is simple, solvent can reuse, it is easy to accomplish industrial production.
Description
Technical field
The invention belongs to nano-powder material fields, and in particular to a kind of preparation method of ceria nanoparticles.
Technical background
At present, countries in the world mainly include preparation, microstructure, macroscopic properties to the research of nanometer metal oxide microparticle
With these aspects of application, wherein the technology of preparing of nanoparticle is crucial, because preparation process and process control are micro- to nanometer
The microstructure and macro property of grain have important influence.The preparation method of nanometer metal oxide microparticle mainly includes chemistry
Method and physical method.Wherein chemical method is divided into infusion process, coprecipitation, homogeneous precipitation method, sol-gel method and microemulsion method again
Deng.Sol-gal process and reverse microemulsion process reaction condition are mild, are easy to control, and equipment investment is small, the particle size of preparation
It is uniformly dispersed controllable, therefore by the favor in industry.
Cerium oxide (CeO2) it is a kind of light rare earth oxide cheap, purposes is extremely wide, have been used for high-performance Ni-H 2 power
Battery, silver-colored leaching agent, Rare Earth Mine clean utilization, methanation catalyst etc..High-performance Ni-MH power cell is universal compared to domestic at present
The automobile-used new energy resource power battery used, with high security, the advantages such as anti-attenuation, low temperature resistant, recyclable, charging rate be fast,
This is applied to pure electric bus field by success, and the development for opening China's light rare earth high-end applications into extensive industry is first
River.Shanghai Science and Technology Univ. develops effective catalyst combination --- and " cerium base catalyst+alcohol catalyst ".Under room temperature, three
Under the concerted catalysis of chlorethanol and rare earth metal cerium, methane conversion is completed.It solves a great problem in organic chemistry, and looks for
Arrived low in cost, conversion efficiently, the mild conversion method of reaction condition, it is contour that this for methane is converted into propellant fuel
Added value chemical products provide new departure, efficiently provide new approaches using peculiar rare earth metal resource for China.
And the performance of rare earth powder body material and its granularity and size have it is important be associated with, work as CeO2The size of powder
Reach Nano grade, is provided with skin effect, bulk effect, dimensional effect and the macroscopical tunnel-effect of nanoparticle, has excellent
Application of micron performance more, therefore, nano Ce O2There is boundless application and development prospect.Investigation of materials work in recent years
Author is to nano Ce O2Preparation method and application carried out a large amount of research, nano Ce O2Preparation have become nano-powder material
One of research hotspot of material.But the nano Ce O of traditional sol-gel method preparation2It is easy to happen reunion, poor dispersion is led
The application performance of product is caused to be deteriorated.Therefore the nano Ce O of partial size controllable precise, good dispersion is developed2Powder preparation method ten
Divide necessity.
Summary of the invention
In view of the drawbacks of the prior art, the purpose of the present invention is to provide a kind of preparation method of ceria nanoparticles,
For solving nano Ce O in the prior art2Reunion is easy to happen in preparation, poor dispersion causes application performance to be deteriorated
Problem.
To achieve the goals above, technical solution provided by the invention are as follows: a kind of preparation method of ceria nanoparticles,
It is characterized by: method includes the following steps:
(1) Ce (NO is weighed3)3﹒ 6H2O is dissolved in deionized water, is configured to aqueous solution;Weigh again complexing agent be dissolved in from
Sub- water, is configured to aqueous solution, and two kinds of solution are mixed, system Ce is made3+Concentration be 1mol/L, and with 25% ammonium hydroxide adjusting pH
To 1-8,30 DEG C of stirring 1h, colloidal sol is formed;
(2) hexamethylene is added into reactor, opens stirring, 60 ± 2 DEG C of temperature of reaction system are controlled, successively to reaction
Colloidal sol made from dropwise addition surfactant, cosurfactant and step (1), colloidal sol are wrapped up by surfactant in device, are formed
Stable colloidal sol-Reverse Microemulsion System;It keeps bath temperature constant, continues 3~6h of stirring, form gel particle;
(3) cooling of gel particle described in step (2) is freezed, filters at low temperature, and -20 DEG C of dehydrated alcohols of use are repeatedly
Washing;
(4) gel particle after step (3) washing is subjected to vacuum drying and removes moisture, can be prepared by presoma;
(5) by presoma high-temperature calcination described in step (4), ceria nanoparticles can be obtained.
The complexing agent is any one of citric acid, tartaric acid, malic acid or polyethylene glycol, and the complexing agent is excellent
It is selected as citric acid or tartaric acid.
The complexing agent and Ce (NO3)3﹒ 6H2The ratio between amount of substance of O is 3~3.2:1.
The surfactant is cetyl trimethylammonium bromide (CTAB), and the cosurfactant is positive fourth
Alcohol.
The mass ratio of the surfactant and hexamethylene is 1:50, the matter of the cosurfactant and hexamethylene
Amount is than being 1:45.
The volume ratio of the colloidal sol and hexamethylene is 3:100.
The temperature that the step 3) gel freezes is 0~-30 DEG C.
The vacuum drying of the step 4) is vacuum freeze drying, and drying temperature is -60~-30 DEG C, and drying time is
24-48h。
The calcination temperature of the step 5) is 400-600 DEG C, time 2-4h.
The preparation method of ceria nanoparticles of the invention, has the advantages that
The present invention utilizes the combination of sol-gel method and reverse microemulsion process, and cerium is allowed to form colloidal sol under complexing agent effect
It is scattered in reverse micro emulsion after presoma, the gelation in " the water core " of surfactant package, the gel particles formed in this way
Diameter is small and controllable, and has surfactant cladding, solves conventional sol gel method micelle in drying and heat treatment and sends out
The problem of stiff reunion, ceria nanoparticles pattern obtained is uniform, size tunable, good dispersion, surface activity are high, and
Preparation process of the present invention is simple, and solvent can reuse, it is easy to accomplish industrial production.
Detailed description of the invention
Fig. 1 is the SEM figure that nano-cerium oxide is made in the embodiment of the present invention 1
Fig. 2 is the flow chart of nano-cerium oxide preparation method of the present invention
Specific embodiment
The flow chart of the nano-cerium oxide preparation method of 1-10 of the embodiment of the present invention is as shown in Figure 2.
Embodiment 1
Weigh 1.085g Ce (NO3)3﹒ 6H2O is dissolved in 1ml deionized water;Citric acid 1.44g is weighed again is dissolved in 1.5ml
Deionized water after mixing two kinds of solution, does not adjust pH value, and 30 DEG C of stirring 1h form colloidal sol;50ml is added into reactor
Hexamethylene opens stirring, controls 60 ± 2 DEG C of temperature of reaction system, and 0.87g cetyl trimethyl is successively added into reactor
Colloidal sol made from ammonium bromide, 1.0ml n-butanol and 1.5ml, colloidal sol are wrapped up by surfactant, form stable colloidal sol-reverse phase
Microemulsion system keeps bath temperature constant, continues to stir 3h, forms gel particle;Gel particle is cooled to 0~-30 DEG C
Freeze, filter at low temperature, and is washed repeatedly with -20 DEG C of dehydrated alcohols;Then vacuum freeze drying is carried out for 24 hours at -60 DEG C,
It can be prepared by presoma;By 500 DEG C of calcining 3h of presoma, nano-cerium oxide can be obtained.It is as shown in Figure 1 to measure SEM figure.Measure oxygen
Change cerium particle diameter distribution is as shown in table 1, and partial size accounts for 90% between 52-82nm.
Embodiment 2
Weigh 1.085g Ce (NO3)3﹒ 6H2O is dissolved in 1ml deionized water;Tartaric acid 1.41g is weighed again is dissolved in 1.5ml
Deionized water after mixing two kinds of solution, does not adjust pH value, and 30 DEG C of stirring 1h form colloidal sol;50ml is added into reactor
Hexamethylene opens stirring, controls 60 ± 2 DEG C of temperature of reaction system, and 0.87g cetyl trimethyl is successively added into reactor
Colloidal sol made from ammonium bromide, 1.0ml n-butanol and 1.5ml, colloidal sol are wrapped up by surfactant, form stable colloidal sol-reverse phase
Microemulsion system keeps bath temperature constant, continues to stir 3h, forms gel particle;Gel particle is cooled to 0~-30 DEG C
Freeze, filter at low temperature, and is washed repeatedly with -20 DEG C of dehydrated alcohols;Then vacuum freeze drying is carried out for 24 hours at -60 DEG C,
It can be prepared by presoma;By 500 DEG C of calcining 3h of presoma, nano-cerium oxide can be obtained.Measure cerium oxide particle diameter distribution such as 1 institute of table
Show, partial size accounts for 90% between 62-98nm.
Embodiment 3
Weigh 1.085g Ce (NO3)3﹒ 6H2O is dissolved in 1ml deionized water;Citric acid 1.44g is weighed again is dissolved in 1.5ml
Deionized water after mixing two kinds of solution, adjusts pH to 5,30 DEG C of stirring 1h with 25% ammonium hydroxide, forms colloidal sol;Into reactor
50ml hexamethylene is added, opens stirring, controls 60 ± 2 DEG C of temperature of reaction system, 0.87g 16 is successively added into reactor
Colloidal sol made from alkyl trimethyl ammonium bromide, 1.0ml n-butanol and 1.5ml, colloidal sol are wrapped up by surfactant, are formed stable
Colloidal sol-Reverse Microemulsion System keeps bath temperature constant, continues to stir 3h, forms gel particle;Gel particle is cooled to
0~-30 DEG C are freezed, and are filtered at low temperature, and are washed repeatedly with -20 DEG C of dehydrated alcohols;Then vacuum refrigeration is carried out at -60 DEG C
Drying for 24 hours, can be prepared by presoma;By 500 DEG C of calcining 3h of presoma, nano-cerium oxide can be obtained.Measure cerium oxide partial size point
Cloth is as shown in table 1, and partial size accounts for 90% between 45-70nm.
Embodiment 4
Weigh 1.085g Ce (NO3)3﹒ 6H2O is dissolved in 1ml deionized water;Citric acid 1.44g is weighed again is dissolved in 1.5ml
Deionized water after mixing two kinds of solution, adjusts pH to 8,30 DEG C of stirring 1h with 25% ammonium hydroxide, forms colloidal sol;Into reactor
50ml hexamethylene is added, opens stirring, controls 60 ± 2 DEG C of temperature of reaction system, 0.87g 16 is successively added into reactor
Colloidal sol made from alkyl trimethyl ammonium bromide, 1.0ml n-butanol and 1.5ml, colloidal sol are wrapped up by surfactant, are formed stable
Colloidal sol-Reverse Microemulsion System keeps bath temperature constant, continues to stir 3h, forms gel particle;Gel particle is cooled to
0~-30 DEG C are freezed, and are filtered at low temperature, and are washed repeatedly with -20 DEG C of dehydrated alcohols;Then vacuum refrigeration is carried out at -60 DEG C
Drying for 24 hours, can be prepared by presoma;By 500 DEG C of calcining 3h of presoma, nano-cerium oxide can be obtained.Measure cerium oxide partial size point
Cloth is as shown in table 1, and partial size accounts for 90% between 40-70nm.
Embodiment 5
Weigh 1.085g Ce (NO3)3﹒ 6H2O is dissolved in 1ml deionized water;Citric acid 1.44g is weighed again is dissolved in 1.5ml
Deionized water after mixing two kinds of solution, adjusts pH to 8,30 DEG C of stirring 1h with 25% ammonium hydroxide, forms colloidal sol;Into reactor
50ml hexamethylene is added, opens stirring, controls 60 ± 2 DEG C of temperature of reaction system, 0.87g 16 is successively added into reactor
Colloidal sol made from alkyl trimethyl ammonium bromide, 1.0ml n-butanol and 1.5ml, colloidal sol are wrapped up by surfactant, are formed stable
Colloidal sol-Reverse Microemulsion System keeps bath temperature constant, continues to stir 4.5h, forms gel particle;Gel particle is cooled down
Freeze to 0~-30 DEG C, filter at low temperature, and is washed repeatedly with -20 DEG C of dehydrated alcohols;Then it is cold that vacuum is carried out at -60 DEG C
Be lyophilized it is dry for 24 hours, can be prepared by presoma;By 500 DEG C of calcining 3h of presoma, nano-cerium oxide can be obtained.Measure cerium oxide partial size
As shown in table 1, partial size accounts for 90% between 25-45nm for distribution.
Embodiment 6
Weigh 1.085g Ce (NO3)3﹒ 6H2O is dissolved in 1ml deionized water;Citric acid 1.44g is weighed again is dissolved in 1.5ml
Deionized water after mixing two kinds of solution, adjusts pH to 8,30 DEG C of stirring 1h with 25% ammonium hydroxide, forms colloidal sol;Into reactor
50ml hexamethylene is added, opens stirring, controls 60 ± 2 DEG C of temperature of reaction system, 0.87g 16 is successively added into reactor
Colloidal sol made from alkyl trimethyl ammonium bromide, 1.0ml n-butanol and 1.5ml, colloidal sol are wrapped up by surfactant, are formed stable
Colloidal sol-Reverse Microemulsion System keeps bath temperature constant, continues to stir 6h, forms gel particle;Gel particle is cooled to
0~-30 DEG C are freezed, and are filtered at low temperature, and are washed repeatedly with -20 DEG C of dehydrated alcohols;Then vacuum refrigeration is carried out at -60 DEG C
Drying for 24 hours, can be prepared by presoma;By 500 DEG C of calcining 3h of presoma, nano-cerium oxide can be obtained.Measure cerium oxide partial size point
Cloth is as shown in table 1, and partial size accounts for 82% between 35-57nm.
Embodiment 7
Weigh 1.085gCe (NO3)3﹒ 6H2O is dissolved in 1ml deionized water;Citric acid 1.54g is weighed again is dissolved in 1.5ml
Deionized water after mixing two kinds of solution, adjusts pH to 8,30 DEG C of stirring 1h with 25% ammonium hydroxide, forms colloidal sol;Into reactor
50ml hexamethylene is added, opens stirring, controls 60 ± 2 DEG C of temperature of reaction system, 0.87g hexadecane is successively added into reactor
Colloidal sol made from base trimethylammonium bromide, 1.0ml n-butanol and 1.5ml, colloidal sol are wrapped up by surfactant, are formed stable molten
Glue-Reverse Microemulsion System keeps bath temperature constant, continues to stir 4.5h, forms gel particle;Gel particle is cooled to
0~-30 DEG C are freezed, and are filtered at low temperature, and are washed repeatedly with -20 DEG C of dehydrated alcohols;Then vacuum refrigeration is carried out at -60 DEG C
Dry 36h, can be prepared by presoma;By 400 DEG C of calcining 4h of presoma, nano-cerium oxide can be obtained.Measure cerium oxide partial size point
Cloth is as shown in table 1, and partial size accounts for 90% between 25-45nm.
Embodiment 8
Weigh 1.085g Ce (NO3)3﹒ 6H2O is dissolved in 1ml deionized water;Citric acid 1.49g is weighed again is dissolved in 1.5ml
Deionized water after mixing two kinds of solution, adjusts pH to 8,30 DEG C of stirring 1h with 25% ammonium hydroxide, forms colloidal sol;Into reactor
50ml hexamethylene is added, opens stirring, controls 60 ± 2 DEG C of temperature of reaction system, 0.87g 16 is successively added into reactor
Colloidal sol made from alkyl trimethyl ammonium bromide, 1.0ml n-butanol and 1.5ml, colloidal sol are wrapped up by surfactant, are formed stable
Colloidal sol-Reverse Microemulsion System keeps bath temperature constant, continues to stir 4.5h, forms gel particle;Gel particle is cooled down
Freeze to 0~-30 DEG C, filter at low temperature, and is washed repeatedly with -20 DEG C of dehydrated alcohols;Then it is cold that vacuum is carried out at -60 DEG C
Dry 48h is lyophilized, can be prepared by presoma;By 600 DEG C of calcining 2h of presoma, nano-cerium oxide can be obtained.Measure cerium oxide partial size
As shown in table 1, partial size accounts for 90% between 25-45nm for distribution.
Embodiment 9
Weigh 1.085g Ce (NO3)3﹒ 6H2O is dissolved in 1ml deionized water;Citric acid 1.44g is weighed again is dissolved in 1.5ml
Deionized water after mixing two kinds of solution, adjusts pH to 8,30 DEG C of stirring 1h with 25% ammonium hydroxide, forms colloidal sol;Into reactor
50ml hexamethylene is added, opens stirring, controls 60 ± 2 DEG C of temperature of reaction system, 0.87g 16 is successively added into reactor
Colloidal sol made from alkyl trimethyl ammonium bromide, 1.0ml n-butanol and 1.5ml, colloidal sol are wrapped up by surfactant, are formed stable
Colloidal sol-Reverse Microemulsion System keeps bath temperature constant, continues to stir 4.5h, forms gel particle;Gel particle is cooled down
Freeze to 0~-30 DEG C, filter at low temperature, and is washed repeatedly with -20 DEG C of dehydrated alcohols;Then it is cold that vacuum is carried out at -60 DEG C
Be lyophilized it is dry for 24 hours, can be prepared by presoma;By 400 DEG C of calcining 3h of presoma, nano-cerium oxide can be obtained.Measure cerium oxide partial size
As shown in table 1, partial size accounts for 90% between 17-45nm for distribution.
Embodiment 10
Weigh 1.085gCe (NO3)3﹒ 6H2O is dissolved in 1ml deionized water;Citric acid 1.44g is weighed again is dissolved in 1.5ml
Deionized water after mixing two kinds of solution, adjusts pH to 8,30 DEG C of stirring 1h with 25% ammonium hydroxide, forms colloidal sol;Into reactor
50ml hexamethylene is added, opens stirring, controls 60 ± 2 DEG C of temperature of reaction system, 0.87g hexadecane is successively added into reactor
Colloidal sol made from base trimethylammonium bromide, 1.0ml n-butanol and 1.5ml, colloidal sol are wrapped up by surfactant, are formed stable molten
Glue-Reverse Microemulsion System keeps bath temperature constant, continues to stir 4.5h, forms gel particle;Gel particle is cooled to
0~-30 DEG C are freezed, and are filtered at low temperature, and are washed repeatedly with -20 DEG C of dehydrated alcohols;Then vacuum refrigeration is carried out at -60 DEG C
Drying for 24 hours, can be prepared by presoma;By 600 DEG C of calcining 3h of presoma, nano-cerium oxide can be obtained.Measure cerium oxide partial size point
Cloth is as shown in table 1, and partial size accounts for 90% between 42-70nm.
Table 1
From test result table 1 as can be seen that ceria nanoparticles average grain diameter prepared by the present invention is in 31.84-
Between 77.16nm, particle diameter distribution is relatively narrow, and there is no agglomerations, and dispersibility is preferably.And by the adjustment of experiment parameter, originally
The ceria nanoparticles of invention preparation can more accurately be controlled between 30-80nm, realize the controllable of particle size interval
Change.
The foregoing is merely preferred embodiments of the invention, are not intended to restrict the invention, for the technology of this field
For personnel, the invention may be variously modified and varied.All any modification, equivalent substitution, improvement and etc. made for the present invention,
It should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of ceria nanoparticles, it is characterised in that: the following steps are included:
(1) Ce (NO is weighed3)3﹒ 6H2O is dissolved in deionized water, is configured to aqueous solution;Complexing agent is weighed again is dissolved in deionization
Water is configured to aqueous solution, and two kinds of solution are mixed, system Ce is made3+Concentration be 1mol/L, with 25% ammonium hydroxide adjust pH to 1~8
Or do not adjust, 30 DEG C of stirring 1h, form colloidal sol;
(2) hexamethylene is added into reactor, opens stirring, controls 60 ± 2 DEG C of temperature of reaction system, successively adds into reactor
Enter colloidal sol made from surfactant, cosurfactant and step (1), colloidal sol is wrapped up by surfactant, formed stable
Colloidal sol-Reverse Microemulsion System;It keeps bath temperature constant, continues 3~6h of stirring, form gel particle;
(3) cooling of gel particle described in step (2) is freezed, filters at low temperature, and washed repeatedly with -20 DEG C of dehydrated alcohols
It washs;
(4) gel particle after step (3) washing is subjected to vacuum drying and removes moisture, can be prepared by presoma;
(5) by presoma high-temperature calcination described in step (4), ceria nanoparticles can be obtained.
2. a kind of preparation method of ceria nanoparticles according to claim 1, it is characterised in that: the complexing agent
For citric acid, tartaric acid and any one of malic acid and polyethylene glycol.
3. a kind of preparation method of ceria nanoparticles according to claim 1, it is characterised in that: the complexing agent
For citric acid or tartaric acid.
4. a kind of preparation method of ceria nanoparticles according to claim 1, it is characterised in that: the complexing agent
With Ce (NO3)3﹒ 6H2The ratio between amount of substance of O is 3~3.2:1.
5. a kind of preparation method of ceria nanoparticles according to claim 1, it is characterised in that: the surface is living
Property agent be cetyl trimethylammonium bromide, the cosurfactant be n-butanol.
6. a kind of preparation method of ceria nanoparticles according to claim 1, it is characterised in that: the surface is living
Property agent and hexamethylene mass ratio be 1:50;The mass ratio of cosurfactant and hexamethylene is 1:45, the colloidal sol and ring
The volume ratio of hexane is 3:100.
7. a kind of preparation method of ceria nanoparticles according to claim 1, it is characterised in that: the step 3) is solidifying
The temperature of jelly knot is 0~-30 DEG C.
8. a kind of preparation method of ceria nanoparticles according to claim 1, it is characterised in that: the step 4)
Vacuum drying is vacuum freeze drying, and drying temperature is -60~-30 DEG C, drying time 24-48h.
9. a kind of preparation method of ceria nanoparticles according to claim 1, it is characterised in that: the step 5)
Calcination temperature is 400-600 DEG C, time 2-4h.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811587542.8A CN109678193B (en) | 2018-12-25 | 2018-12-25 | Preparation method of nano cerium oxide particles |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811587542.8A CN109678193B (en) | 2018-12-25 | 2018-12-25 | Preparation method of nano cerium oxide particles |
Publications (2)
Publication Number | Publication Date |
---|---|
CN109678193A true CN109678193A (en) | 2019-04-26 |
CN109678193B CN109678193B (en) | 2021-06-15 |
Family
ID=66189199
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201811587542.8A Active CN109678193B (en) | 2018-12-25 | 2018-12-25 | Preparation method of nano cerium oxide particles |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN109678193B (en) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110255599A (en) * | 2019-07-11 | 2019-09-20 | 河北铭万精细化工有限公司 | A kind of preparation method of nano cerium oxide powder |
CN112490475A (en) * | 2020-10-28 | 2021-03-12 | 西安交通大学 | Method for synthesizing electrolyte powder based on complexation-freeze drying method and obtained electrolyte powder |
CN113428888A (en) * | 2020-03-23 | 2021-09-24 | 厦门稀土材料研究所 | High-dispersion cerium oxide nano sol and preparation method and application thereof |
CN113877563A (en) * | 2021-10-27 | 2022-01-04 | 山东金海钛业资源科技有限公司 | Cerium-coated titanium dioxide and preparation method thereof |
CN114149021A (en) * | 2021-12-09 | 2022-03-08 | 柯子星 | Method for preparing nano cerium from oriental beauty tea extract and application |
CN114958208A (en) * | 2022-07-07 | 2022-08-30 | 中国科学院长春光学精密机械与物理研究所 | Super-smooth magnetorheological polishing solution and preparation method thereof |
CN116251562A (en) * | 2023-02-10 | 2023-06-13 | 广州市汉宵科研技术有限公司 | Nanoscale cerium oxide particle material and preparation method thereof |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101279719A (en) * | 2008-03-21 | 2008-10-08 | 北京理工大学 | Preparation for nano-oxide powder |
CN101880154A (en) * | 2010-06-25 | 2010-11-10 | 沈阳大学 | Preparation method of nanometer cordierite-based ceramic dielectric material used for high-frequency chip inductor |
CN102942205A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Morphology controllable nanometer CeO2 preparation method |
CN104163444A (en) * | 2014-07-18 | 2014-11-26 | 西南科技大学 | Alpha-alumina hollow ball preparation method |
CN105618032A (en) * | 2016-01-19 | 2016-06-01 | 中国建筑材料科学研究总院 | Supported manganese based low-temperature denitration catalyst and preparation method thereof |
CN105819497A (en) * | 2016-03-09 | 2016-08-03 | 大连理工大学 | Preparation method of tin dioxide nanoparticles |
CN107117635A (en) * | 2017-06-28 | 2017-09-01 | 苏州纳迪微电子有限公司 | A kind of preparation method of ball-aluminium oxide powder |
-
2018
- 2018-12-25 CN CN201811587542.8A patent/CN109678193B/en active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101279719A (en) * | 2008-03-21 | 2008-10-08 | 北京理工大学 | Preparation for nano-oxide powder |
CN101880154A (en) * | 2010-06-25 | 2010-11-10 | 沈阳大学 | Preparation method of nanometer cordierite-based ceramic dielectric material used for high-frequency chip inductor |
CN102942205A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Morphology controllable nanometer CeO2 preparation method |
CN104163444A (en) * | 2014-07-18 | 2014-11-26 | 西南科技大学 | Alpha-alumina hollow ball preparation method |
CN105618032A (en) * | 2016-01-19 | 2016-06-01 | 中国建筑材料科学研究总院 | Supported manganese based low-temperature denitration catalyst and preparation method thereof |
CN105819497A (en) * | 2016-03-09 | 2016-08-03 | 大连理工大学 | Preparation method of tin dioxide nanoparticles |
CN107117635A (en) * | 2017-06-28 | 2017-09-01 | 苏州纳迪微电子有限公司 | A kind of preparation method of ball-aluminium oxide powder |
Non-Patent Citations (1)
Title |
---|
段国荣等: "溶胶-乳液蒸馏法制备纳米氧化锆超细粉", 《科技创新导报》 * |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110255599A (en) * | 2019-07-11 | 2019-09-20 | 河北铭万精细化工有限公司 | A kind of preparation method of nano cerium oxide powder |
CN110255599B (en) * | 2019-07-11 | 2022-02-01 | 河北铭万精细化工有限公司 | Preparation method of nano cerium oxide powder |
CN113428888A (en) * | 2020-03-23 | 2021-09-24 | 厦门稀土材料研究所 | High-dispersion cerium oxide nano sol and preparation method and application thereof |
CN112490475A (en) * | 2020-10-28 | 2021-03-12 | 西安交通大学 | Method for synthesizing electrolyte powder based on complexation-freeze drying method and obtained electrolyte powder |
CN113877563A (en) * | 2021-10-27 | 2022-01-04 | 山东金海钛业资源科技有限公司 | Cerium-coated titanium dioxide and preparation method thereof |
CN114149021A (en) * | 2021-12-09 | 2022-03-08 | 柯子星 | Method for preparing nano cerium from oriental beauty tea extract and application |
CN114149021B (en) * | 2021-12-09 | 2024-02-06 | 柯子星 | Method for preparing nano cerium from eastern beauty tea extract and application of nano cerium |
CN114958208A (en) * | 2022-07-07 | 2022-08-30 | 中国科学院长春光学精密机械与物理研究所 | Super-smooth magnetorheological polishing solution and preparation method thereof |
CN116251562A (en) * | 2023-02-10 | 2023-06-13 | 广州市汉宵科研技术有限公司 | Nanoscale cerium oxide particle material and preparation method thereof |
Also Published As
Publication number | Publication date |
---|---|
CN109678193B (en) | 2021-06-15 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN109678193A (en) | A kind of preparation method of ceria nanoparticles | |
CN103011306B (en) | Method for preparing nanometer-level cube-like cobaltosic oxide | |
CN103474645B (en) | The preparation method of lithium titanate | |
CN106410226A (en) | Graphene-doped modified nano-perovskite-type La(1-x)SrxMnO3 composite material as well as preparation method and application of composite material | |
CN105060351B (en) | Flower-like cobaltosic oxide material composed of nanoparticles and preparation method thereof | |
CN101113010A (en) | Method for preparing cerium oxide nano particle by auxiliary microwave | |
CN102139923A (en) | Method for preparing molybdenum trioxide material with orthorhombic phase single crystal nano belt structure | |
CN109626447A (en) | Nickelic anode material for lithium-ion batteries of a kind of concentration gradient magnesium doping and preparation method thereof | |
CN112794369B (en) | Preparation method and application of nano lithium cobalt oxide positive electrode material | |
CN103435097B (en) | Preparation method and application of nano zirconia | |
CN105406058B (en) | A kind of preparation method of super large particle diameter nickel cobalt aluminum oxide | |
CN110203976A (en) | Rapid synthesis flakes ZnCo2O4The preparation method of-ZnO compound electric grade material | |
CN105329932B (en) | Method for large-scale preparation of carbon-doped mixed transition metal oxide porous microspheres | |
CN107857300B (en) | A kind of preparation method of β type bismuth oxide | |
CN101767997B (en) | Method for preparing NiTiO3 nano-powder by sol-gel | |
CN102962470B (en) | Method for preparing spherical ultrafine nickel powder at room temperature | |
CN105271443B (en) | Method for preparing flaky nano CoO or Co3O4 through assistant microwave heating | |
CN106340642A (en) | Long-circulation and high-capacity lithium battery positive electrode material and preparing method | |
CN103058259A (en) | Preparation method for chestnut-shaped copper sulphide hollow micron sphere composed of nanosheets | |
CN107293410B (en) | A kind of CeO2The preparation method of the porous composite nano-microspheres of/Ni/NiO | |
CN108101123A (en) | Four-prism vanadic acid nickel nano material and preparation method thereof | |
CN104030341A (en) | Preparation method of copper oxide nanomaterial | |
CN101983927B (en) | Preparation method of hollow yttrium oxide micro/nanospheres | |
CN106992285B (en) | A kind of preparation method of nickel cobalt aluminium ternary precursor | |
CN102795659B (en) | Method for preparing rod-like zinc oxide nano-crystals |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |