CN101792171B - Preparation method of cerium oxide nanoballs - Google Patents
Preparation method of cerium oxide nanoballs Download PDFInfo
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- CN101792171B CN101792171B CN2010101175823A CN201010117582A CN101792171B CN 101792171 B CN101792171 B CN 101792171B CN 2010101175823 A CN2010101175823 A CN 2010101175823A CN 201010117582 A CN201010117582 A CN 201010117582A CN 101792171 B CN101792171 B CN 101792171B
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Abstract
The invention relates to a preparation method of cerium oxide nanoballs, and belongs to the technical field of the preparation processes of the inorganic nanomaterials. The key points of the method of the invention include: stirring and mixing cerium salt and a certain amount of surfactant at room temperature, dissolving the mixture in a mixed solution of water and an organic solvent and ultrasonically processing the mixture for 5 to 10 minutes, wherein the cerium salt is optimally cerium nitrate; the surfactant is most preferably polyvinylpyrrolidone; and the belonged organic solvent is most preferably diglycol; then transferring the mixed solution into a high pressure reaction kettle to perform a solvothermal reaction; heating the mixed solution to perform reaction for 24 to 28 hours at the temperature of 100 to 200 DEG C so as to obtain the cerium oxide nanoball sol; evaporating the sol at the temperature of 1500 o 180 DEG C to dryness; and forging the obtained powder for 1 to 4 hours at the temperature of 400 to 600 DEG C; and finally obtaining the cerium oxide nanoballs in the shape of yellow solid powder. The nanoballs have a particle size ranging from 30 to 160nm and high performance and can be applied in fields of ultraviolet light shielding, mechanical polishing and automobile exhaust catalyzation and the like.
Description
Technical field
The present invention relates to a kind of preparation method of cerium oxide nanoballs, belong to the inorganic nano material preparation process technology field.
Background technology
Rare earth material thereby is also referred to as " treasure-house " of novel material because performances such as the electricity of its uniqueness, light, heat, magnetic are having a wide range of applications aspect high energy magnetic device, luminescent device, catalyzer and other functional materialss.The rare earth resources of China is very abundant, accounts for the world's more than 80% of proven reserve, and industrial reserves is the first in the world, for the development of China's rare-earth industry provides advantageous condition.As a kind of important rare-earth nano oxide, cerium oxide is widely used in fields such as purifying vehicle exhaust, chemically machinery polished, fuel cell because of having good oxygen storage capacity and special structure.
Along with going deep into of nanotechnology research, the cerium oxide low-dimensional nano structure has been subjected to people's attention because of advantages such as its specific surface area is big, good dispersity, anisotropy, catalytic activity height.The spherical cerium oxide microstructure that people attempt adopting the whole bag of tricks design to synthesize variform: Chinese patent CN1699282 has proposed the preparation method of monodisperse spherical cerium oxide, but its gained cerium oxide ball has reached submicron (300nm) more greatly for precipitation and particle diameter; Chinese patent CN101117233 has proposed the preparation method of meso-porous cerium dioxide micro-balloon, the also bigger and pattern heterogeneity of particle diameter of the mesoporous ball of gained precipitation shape cerium dioxide; Chinese patent CN1371867A has proposed a kind of preparation method of cerium oxide sol, but this law part harshness, complex procedures, the cerium oxide particle size inequality (6～200nm) that obtains; Chinese patent CN101092246A has proposed a kind of method for preparing cerium oxide sol, and this method program is loaded down with trivial details, and what obtain in addition is cerium oxide particle; Document (Jimmy C.Yu, et al.Chem.Mater.2005,17,4514-4520) reported a kind of method for preparing cerium oxide nanoballs, but gained all is that precipitation shape cerium dioxide ball and size are uncontrollable; In addition, though document (Daniel Andreescu, et al.Colloids and Surfaces A:Physicochem.Eng.Aspects 2006,291,93-100) reported a kind of preparation method of gluey cerium oxide ball, but the cerium oxide ball particle of gained is bigger, particle diameter is 1～3 μ m.In sum, effectively synthetic particle diameter cerium oxide nanoballs less, that size is controlled, that stability is good has certain challenge.
Summary of the invention:
The preparation method who the purpose of this invention is to provide a kind of cerium oxide nanoballs.Another purpose of the present invention provides that a kind of technology is simple, the cerium oxide nanoballs colloidal sol preparation method of excellent property.
The present invention is a kind of preparation method of cerium oxide nanoballs, it is characterized in that having following process and step:
A, a certain amount of cerium salt and certain amount of surfactant are mixed in stirring at room, and it is dissolved in the mixed solution of water and organic solvent supersound process 5～10min; The mass ratio of used tensio-active agent and cerium salt is 1: 0.5～1: 3.0; Water is 1: 0.3～1/3.0 with the volume of organic solvent ratio; Described cerium salt is any in cerous nitrate, cerous sulfate, the Cerium II Chloride; Described tensio-active agent is any in polyoxyethylene glycol, the polyvinylpyrrolidone; Described organic solvent is any in glycol ether, the ethylene glycol;
B, above-mentioned solution is transferred to carries out solvent thermal reaction in the autoclave then, behind reacting by heating 24～48h under 100～200 ℃ of conditions, naturally cooling obtains the cerium oxide nanoballs colloidal sol of stable homogeneous;
C, then with above-mentioned colloidal sol behind 150～180 ℃ of following evaporates to dryness, with the powder of gained 400～600 ℃ down behind calcining 1～4h both the Powdered cerium oxide nanoballs of yellow solid.
Described cerium salt is optimum to be cerous nitrate; Described tensio-active agent is optimum to be polyvinylpyrrolidone; Described organic solvent is optimum to be glycol ether.
The inventive method characteristics and advantage as described below:
(1), the colloidal sol of gained is more stable, at room temperature long-term storage can be stabilized in more than 3 months.
(2), the cerium oxide nanoballs good dispersity of gained, particle diameter be less, at 30～160nm; In addition, the structure properties of cerium oxide nanoballs is good.
(3), the inventive method technology is simple and stable, easy to operate; Can regulate and control particle diameter by temperature of reaction and reaction times.
(4), the cerium oxide nanoballs of gained of the present invention, can be applicable to aspects such as ultravioletlight screening, automotive exhaust catalysis, mechanical polishing.
Description of drawings
Fig. 1 is transmission electron microscope (TEM) photo of the embodiment of the invention 1 gained sample.
Fig. 2 is scanning electron microscope (SEM) photo of the embodiment of the invention 2 gained samples.
Fig. 3 is transmission electron microscope (TEM) photo of the embodiment of the invention 3 gained samples.
Fig. 4 is transmission electron microscope (TEM) photo of the embodiment of the invention 4 gained samples.
Embodiment
After now specific embodiments of the invention being described in.
Embodiment 1
Cerous nitrate and the 0.5g polyvinylpyrrolidone stirring at room 5min of 2mmol are dissolved in the 10mL water, add the 30mL glycol ether then, stirring 5min transfers to after mixing in the 50mL autoclave, leave standstill 24h under 180 ℃ of conditions, promptly obtain the cerium oxide nanoballs colloidal sol of stable stable homogeneous behind the naturally cooling, behind 180 ℃ of evaporates to dryness, calcine 2h down at 500 ℃ again, obtain yellow oxidation cerium nanometer ball pressed powder.
Embodiment 2
Cerous nitrate and the ultrasonic 5min of 4g polyvinylpyrrolidone room temperature of 2mmol are dissolved in the 10mL water, add the 30mL glycol ether then, after mixing, ultrasonic 5min is transferred in the 50mL autoclave, leave standstill 24h under 180 ℃ of conditions, promptly obtain the cerium oxide nanoballs colloidal sol of stable homogeneous behind the naturally cooling; Behind 150 ℃ of evaporates to dryness, calcine 1h down at 600 ℃, obtain yellow oxidation cerium nanometer ball pressed powder.
Embodiment 3
Cerium II Chloride and the ultrasonic 5min of 0.5g polyvinylpyrrolidone room temperature of 2mmol are dissolved in the 15mL water, add the 25mL glycol ether then, after mixing, ultrasonic 5min is transferred in the 50mL autoclave, leave standstill 24h under 120 ℃ of conditions, promptly obtain the cerium oxide nanoballs colloidal sol of stable homogeneous behind the naturally cooling; Behind 170 ℃ of evaporates to dryness, calcine 3h down at 450 ℃, obtain yellow oxidation cerium nanometer ball pressed powder.
Embodiment 4
Cerium II Chloride and the ultrasonic 5min of 1.0g polyvinylpyrrolidone room temperature of 1.5mmol are dissolved in the 30mL water, add the 10mL glycol ether then, after mixing, ultrasonic 5min is transferred in the 50mL autoclave, leave standstill 24h under 180 ℃ of conditions, promptly obtain the cerium oxide nanoballs colloidal sol of stable homogeneous behind the naturally cooling; Behind 180 ℃ of evaporates to dryness, calcine 2h down at 500 ℃, obtain yellow oxidation cerium nanometer ball pressed powder.
Detection test to the gained sample
(1), the transmission electron microscope (TEM) of gained sample is measured in the example 1.
Referring to Fig. 1, Fig. 1 (a) is the TEM photo before the test sample calcining in the example 1, and Fig. 1 (b) is the TEM photo after the test sample calcining in the example 1, as can be seen from Figure 1, the cerium oxide nanoballs particle diameter is 80-110nm, good dispersity, and pattern does not change before and after the calcining.
(2), the scanning electronic microscope (SEM) of gained sample is measured in the example 2.
Referring to Fig. 2, Fig. 2 is the SEM photo of test sample in the example 2, and as can be seen from Figure 2, the cerium oxide nanoballs particle diameter is 40～150nm.
(3), the transmission electron microscope (TEM) of gained sample is measured in the example 3.
Referring to Fig. 3, Fig. 3 is the TEM photo of test sample in the example four, and as can be seen from Figure 3, the cerium oxide nanoballs particle diameter is 30-80nm.
(4), the transmission electron microscope (TEM) of gained sample is measured in the example 4.
Referring to Fig. 4, Fig. 4 is the TEM photo of test sample in the example four, and as can be seen from Figure 4, the cerium oxide nanoballs particle diameter is 30-70nm.
Claims (2)
1. the preparation method of a cerium oxide nanoballs is characterized in that having following process and step:
A, a certain amount of cerium salt and certain amount of surfactant are mixed in stirring at room, and it is dissolved in the mixed solution of water and organic solvent supersound process 5～10min; The mass ratio of used tensio-active agent and cerium salt is 1: 0.5～1: 3.0; Water is 1: 0.3～1: 3.0 with the volume of organic solvent ratio; Described cerium salt is any in cerous nitrate, cerous sulfate, the Cerium II Chloride; Described tensio-active agent is any in polyoxyethylene glycol, the polyvinylpyrrolidone; Described organic solvent is any in glycol ether, the ethylene glycol;
B, above-mentioned solution is transferred to carries out solvent thermal reaction in the autoclave then, behind reacting by heating 24～48h under 100～200 ℃ of conditions, naturally cooling obtains the cerium oxide nanoballs colloidal sol of stable homogeneous;
C, then with above-mentioned colloidal sol behind 150～180 ℃ of following evaporates to dryness, the powder of gained is promptly being got the Powdered cerium oxide nanoballs of yellow solid behind calcining 1～4h down at 400～600 ℃.
2. the preparation method of a kind of cerium oxide nanoballs according to claim 1 is characterized in that described cerium salt is optimum and is cerous nitrate; Described tensio-active agent is optimum to be polyvinylpyrrolidone; Described organic solvent is optimum to be glycol ether.
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| US6677262B2 (en) * | 2000-07-05 | 2004-01-13 | Shin-Etsu Chemical Co., Ltd. | Rare earth oxide, basic rare earth carbonate, making method, phosphor, and ceramic |
| CN100480166C (en) * | 2003-09-28 | 2009-04-22 | 中国科学院化学研究所 | Nano composite inorganic semiconductor hollow ball and preparation method thereof |
| CN1288088C (en) * | 2004-06-03 | 2006-12-06 | 中南大学 | Process for preparing high purity active nano ceria |
| CN1297479C (en) * | 2004-08-17 | 2007-01-31 | 山东师范大学 | Preparation method of nanometer ball |
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