CN102849774A - Method for preparing nanometer cerium oxide by hydrothermal method - Google Patents
Method for preparing nanometer cerium oxide by hydrothermal method Download PDFInfo
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- CN102849774A CN102849774A CN2012100059294A CN201210005929A CN102849774A CN 102849774 A CN102849774 A CN 102849774A CN 2012100059294 A CN2012100059294 A CN 2012100059294A CN 201210005929 A CN201210005929 A CN 201210005929A CN 102849774 A CN102849774 A CN 102849774A
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- cerium oxide
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Abstract
The invention provides a method for preparing nanometer cerium oxide. The invention adopts the following technical scheme that the method comprises the following steps: 1) preparing a Ce(NO3)3.6H2O aqueous solution with a concentration of 0.05-0.1 mol/L at room temperature; 2) taking a certain volume of the Ce(NO3)3.6H2O aqueous solution at room temperature, dropwisely adding undiluted commercially-available 25% ammonia water into the Ce(NO3)3.6H2O aqueous solution according to a volume ratio of 10:1-3; 3) allowing the mixed solution to react for 2-24 hours, after the reaction, performing centrifugation, removing the liquid at the upper level, washing the powder obtained after centrifugation, and drying to obtain solid powder. The invention realizes one-step synthesis of nanometer cerium oxide by a hydrothermal method; the preparation process is simple, and the requirements for production equipment and process conditions are low; no organic solvent is added, which is basically free of pollution, and is quite environment-friendly; no macromolecular surfactant is added, which prevents posttreatment process such as washing and the like; the kinds of the required raw materials are few, and when compared with traditional process, the method of the invention is quite low in production cost; the method cam prepare uniform and pure cerium oxide nanoparticles, cerium oxide nanorods, and mixtures of the above two.
Description
Technical field
The invention belongs to technical field of material, particularly a kind of hydrothermal method prepares the method for cerium oxide nano particle nanometer rod and composition thereof.
Background technology
Rare-earth nano oxide has important application at aspects such as high technology ceramics, photocell, magnetic recording and sensor, catalyzer, luminescent materials.Wherein to have a crystal formation single for nano ceric oxide, the advantage such as electric property and optical property are good and be able to widespread use.Current its range of application expands to purifying vehicle exhaust catalytic material, high temperature oxygen-sensitive material, pH sensing material, Solid Oxide Fuel Cell (SOFC) electrode materials, electrochemical reaction and promotes the modern high-tech field such as the coated material of material, chemically machinery polished (CMP) abrasive substance and metal oxidation resistance and corrosion and additive from fields such as luminescent material, glass polishing agent, catalyzer, electronic ceramics, uv-absorbing agents.
At present the main method of preparation nano-cerium oxide has solid phase method, liquid phase method and vapor phase process, especially liquid phase method because of have equipment simple, need not the advantages such as harsh physical condition, easy amplification such as high vacuum and become the present the most frequently used method of nano-cerium oxide for preparing.Up to now, the investigator has synthesized the CeO of different-shape and size
2, such as nanotube, bar-shaped, wire, petal-shaped etc.Wherein the one dimension cerium oxide nano materials such as nano wire, nanometer rod etc., becomes the focus of current research owing to its purposes at aspects such as the micro-nano devices of sensor.Present chemical preparation process comprises the precipitator method, sol-gel method, hydrothermal method and microemulsion method etc. can make the bar-shaped cerium oxide of 1-dimention nano, but these methods have the prescription complexity, generally need to add the tensio-active agent that is fit to, the harsh and high in cost of production shortcoming of working condition.Thereby it is simple to develop a kind of prescription, and processing condition require low and can obtain functional, as to have monodispersity 1-dimention nano cerium oxide manufacture method, and higher nanometer rod productivity is arranged, and are significant.
Summary of the invention
The object of the present invention is to provide a kind of working condition requirement simple, prepare cheaply the method for nano-cerium oxide.
For this reason, the present invention adopts following technical scheme:
The step of the method is as follows:
1) Ce (NO of preparation 0.05-0.1mol/L under the room temperature
3)
36H
2The O aqueous solution;
2) room temperature is got the Ce (NO of certain volume
3)
36H
2The O aqueous solution drips commercially available 25% ammoniacal liquor of not diluted to Ce (NO according to volume ratio 10:1-3
3)
36H
2In the O aqueous solution;
3) above-mentioned mixed solution reaction is 2-24 hour, and it is centrifugal that reaction finishes rear taking-up, removes supernatant liquid, with centrifugal gained powder washing, is dried to pressed powder.
By above technical scheme, the present invention has following technique effect:
1. the nano-cerium oxide that adopted the hydrothermal method one-step synthesis, this preparation technology is simple, and production unit and processing condition require low;
2. do not add any organic solvent, substantially pollution-free, very environmental protection; Do not add molecules surfactant and avoided the aftertreatment technologys such as washing;
3. the desired raw material kind is few, and the traditional technology production cost is very low relatively;
4. the method can make evenly pure cerium oxide nano particle, cerium oxide nano-rod and composition thereof.
The method is especially at Ce (NO
3)
36H
2The O aqueous solution and ammoniacal liquor volume ratio 10:3 or at pH value greater than the cerium oxide nano-rod that can make the high size uniform of purity at 12 o'clock.The method has avoided traditional liquid phase method desired raw material many simultaneously, complex process, and working condition requires harsh, needs to add organic surface active agent and needs with processes such as organic reagent wash.The processing condition gentleness is controlled, and is environment friendly and pollution-free, and comparing traditional preparation method has huge progress and productive value.
?
Description of drawings
Accompanying drawing is scanning electron microscope (SEM) and transmission electron microscope (TEM) photo of prepared cerium oxide nano-powder.
Fig. 1 is transmission electron microscope (TEM) photo of the cerium oxide nano particle of embodiment 1 preparation;
Fig. 2 is the cerium oxide nano particle of embodiment 2 preparations and scanning electron microscope (SEM) photo of nanometer rod mixed powder;
Fig. 3 is scanning electron microscope (SEM) photo of the cerium oxide nano-rod of embodiment 3 preparations.
Embodiment
The material mixture ratio that present embodiment adopts uses:
Purity is 98.0% Ce (NO
3)
36H
2O;
Concentration is 25.0% ammoniacal liquor.
Ce (NO
3)
36H
2When the O aqueous solution and ammoniacal liquor volume ratio 10:1, the product that makes is cerium oxide nano particle;
Ce (NO
3)
36H
2When the O aqueous solution and ammoniacal liquor volume ratio 10:2, the product that makes is the mixture of cerium oxide nano particle and nanometer rod;
Ce (NO
3)
36H
2When the O aqueous solution and ammoniacal liquor volume ratio 10:3, the product that makes is cerium oxide nano-rod.
Embodiment 1:
1) Ce (NO of preparation 0.05mol/L under the room temperature
3)
36H
2The O aqueous solution;
2) room temperature is got the Ce (NO of 91mL
3)
36H
2The O aqueous solution places flask, under the magnetic agitation, drips 9.1mL ammoniacal liquor in flask;
3) above-mentioned mixed solution reacts under magnetic agitation, gets respectively each 1mL of mixing solutions when reaction finished in 2 hours, 8 hours to 24 hours, with materials centrifugally, remove supernatant liquid.Centrifugal gained powder is gone out washing with pure water, then place loft drier to be dried to pressed powder, use transmission electron microscope observing, find that the product that makes is that particle diameter is the cerium oxide nano particle of 10-30nm, see accompanying drawing 1.
Embodiment 2:
1) Ce (NO of preparation 0.08mol/L under the room temperature
3)
36H
2The O aqueous solution;
2) room temperature is got the Ce (NO of 83mL
3)
36H
2The O aqueous solution places flask, under the magnetic agitation, drips 16.6mL ammoniacal liquor in flask;
3) above-mentioned mixed solution reacts under magnetic agitation respectively in reaction, gets respectively each 1mL of mixing solutions when reaction finished in 2 hours, 8 hours to 24 hours, with materials centrifugally, remove supernatant liquid.Centrifugal gained powder is gone out washing with pure water, then place loft drier to be dried to pressed powder, use field emission microscopy observation, the product that discovery makes is that particle diameter is the mixture of the nanometer rod of the cerium oxide nano particle of 10-30nm and diameter 10-30nm, length 100-300nm, sees accompanying drawing 2.
Embodiment 3:
1) Ce (NO of preparation 0.1mol/L under the room temperature
3)
36H
2The O aqueous solution;
2) room temperature is got the Ce (NO of 77mL
3)
36H
2The O aqueous solution places flask, under the magnetic agitation, drips 23.1mL ammoniacal liquor in flask;
3) above-mentioned mixed solution reacts under magnetic agitation respectively in reaction, gets respectively each 1mL of mixing solutions when reaction finished in 2 hours, 8 hours to 24 hours, with materials centrifugally, remove supernatant liquid.Centrifugal gained powder is gone out washing with pure water, then place loft drier to be dried to pressed powder, use field emission microscopy observation, find that the product that makes is the nanometer rod of diameter 10-30nm, length 100-300nm, see accompanying drawing 3.
Embodiment 4:
1) Ce (NO of preparation 0.05mol/L under the room temperature
3)
36H
2The O aqueous solution;
2) room temperature is got the Ce (NO of 77mL
3)
36H
2The O aqueous solution places flask, under the magnetic agitation, drips 23.1mL ammoniacal liquor in flask;
3) above-mentioned mixed solution reacted 2 hours under magnetic agitation, and reaction product is centrifugal, removed supernatant liquid.Centrifugal gained powder is washed with pure water, then place loft drier to be dried to pressed powder, the product that makes is that diameter is 10～30nm, and length reaches the cerium oxide nano-rod of 150～300nm.
Embodiment 5:
1) Ce (NO of preparation 0.1mol/L under the room temperature
3)
36H
2The O aqueous solution;
2) room temperature is got the Ce (NO of 91mL
3)
36H
2The O aqueous solution places flask, under the magnetic agitation, drips 9.1mL ammoniacal liquor in flask;
3) above-mentioned mixed solution reacted 2 hours under magnetic agitation, and reaction product is centrifugal, removed supernatant liquid.Centrifugal gained powder is gone out washing with pure water, then place loft drier to be dried to pressed powder, the product that makes is that particle diameter is the cerium oxide nano particle of 10-30nm.
Embodiment 6:
1) Ce (NO of preparation 0.08mol/L under the room temperature
3)
36H
2The O aqueous solution;
2) room temperature is got the Ce (NO of 91mL
3)
36H
2The O aqueous solution places flask, under the magnetic agitation, drips 9.1mL ammoniacal liquor in flask;
3) above-mentioned mixed solution reacted 2 hours under magnetic agitation, and reaction product is centrifugal, removed supernatant liquid.Centrifugal gained powder is gone out washing with pure water, then place loft drier to be dried to pressed powder, the product that makes is that particle diameter is the cerium oxide nano particle of 10-30nm.
Embodiment 7:
1) Ce (NO of preparation 0.08mol/L under the room temperature
3)
36H
2The O aqueous solution;
2) room temperature is got the Ce (NO of 77mL
3)
36H
2The O aqueous solution places flask, under the magnetic agitation, drips 23.1mL ammoniacal liquor in flask;
3) above-mentioned mixed solution reacted 2 hours under magnetic agitation, and reaction product is centrifugal, removed supernatant liquid.Centrifugal gained powder is gone out washing with pure water, then place loft drier to be dried to pressed powder, the product that makes is that diameter is 10～30nm, and length reaches the cerium oxide nano-rod of 150～300nm.
From embodiment 2,3,4,7 as seen, when at Ce (NO
3)
36H
2The O aqueous solution and ammoniacal liquor volume ratio 10:3 or at pH value greater than the cerium oxide nano-rod that can make the high size uniform of purity at 12 o'clock, and purity is more than 95%, come compared with traditional method, the convenient convenience of this kind method, speed of response is fast than traditional method, the nanometer rod diameter that obtains is 10～30nm, and length reaches the higher economic worth of having of 150～300nm.
Claims (4)
1. a hydrothermal method prepares the method for nano-cerium oxide, it is characterized in that the step of the method is as follows:
1) Ce (NO of preparation 0.05-0.1mol/L under the room temperature
3)
36H
2The O aqueous solution;
2) room temperature is got the Ce (NO of certain volume
3)
36H
2The O aqueous solution drips commercially available 25% ammoniacal liquor of not diluted to Ce (NO according to volume ratio 10:1-3
3)
36H
2In the O aqueous solution;
3) above-mentioned mixed solution reaction is 2-24 hour, and it is centrifugal that reaction finishes rear taking-up, removes supernatant liquid, with centrifugal gained powder washing, is dried to pressed powder.
2. a kind of hydrothermal method as claimed in claim 1 prepares the method for nano-cerium oxide, it is characterized in that: Ce (NO
3)
36H
2When the O aqueous solution and ammoniacal liquor volume ratio 10:1, the pressed powder that makes is cerium oxide nano particle.
3. a kind of hydrothermal method as claimed in claim 1 prepares the method for nano-cerium oxide, it is characterized in that: Ce (NO
3)
36H
2When the O aqueous solution and ammoniacal liquor volume ratio 10:2, the pressed powder that makes is the mixture of cerium oxide nano particle and nanometer rod.
4. a kind of hydrothermal method as claimed in claim 1 prepares the method for nano-cerium oxide, it is characterized in that: Ce (NO
3)
36H
2When the O aqueous solution and ammoniacal liquor volume ratio 10:3, the pressed powder that makes is cerium oxide nano-rod.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274441A (en) * | 2013-05-23 | 2013-09-04 | 浙江理工大学 | Method for preparing nanoscale sheet cerium oxide by hydrothermal method |
| CN105565360A (en) * | 2016-02-29 | 2016-05-11 | 哈尔滨理工大学 | Method for synthesizing and controlling cerium dioxide micro-nano structure and morphology by hydrothermal process |
| CN109794277A (en) * | 2019-01-30 | 2019-05-24 | 扬州工业职业技术学院 | A kind of ceria/graphite phase carbon nitride composite material and its application in photocatalysis |
| CN110743543A (en) * | 2019-10-25 | 2020-02-04 | 李家宝 | Three-way catalyst |
| CN110918081A (en) * | 2019-12-04 | 2020-03-27 | 吉林省电力科学研究院有限公司 | Plasma cerium oxide catalyst and preparation method thereof |
| CN112467154A (en) * | 2020-12-03 | 2021-03-09 | 福州大学 | Preparation method of cerium oxide loaded nickel-iron catalyst |
| WO2023125890A1 (en) * | 2021-12-30 | 2023-07-06 | 安集微电子科技（上海）股份有限公司 | Method for synthesizing cerium oxide, cerium oxide, and chemical mechanical polishing solution |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101633513A (en) * | 2008-07-25 | 2010-01-27 | 中国科学院研究生院 | Method for preparing cerium hydroxide nano rod |
| CN102050479A (en) * | 2011-01-27 | 2011-05-11 | 山东交通学院 | Ceric oxide nanorod and preparation method thereof |
| CN102285678A (en) * | 2011-06-09 | 2011-12-21 | 北京大学 | Method for preparing cerium oxide nano particles and antioxidation use thereof |
-
2012
- 2012-01-10 CN CN2012100059294A patent/CN102849774A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101633513A (en) * | 2008-07-25 | 2010-01-27 | 中国科学院研究生院 | Method for preparing cerium hydroxide nano rod |
| CN102050479A (en) * | 2011-01-27 | 2011-05-11 | 山东交通学院 | Ceric oxide nanorod and preparation method thereof |
| CN102285678A (en) * | 2011-06-09 | 2011-12-21 | 北京大学 | Method for preparing cerium oxide nano particles and antioxidation use thereof |
Non-Patent Citations (1)
| Title |
|---|
| 乐琳: "不同粒径CeO2纳米粒子的控制合成", 《光谱实验室》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103274441A (en) * | 2013-05-23 | 2013-09-04 | 浙江理工大学 | Method for preparing nanoscale sheet cerium oxide by hydrothermal method |
| CN105565360A (en) * | 2016-02-29 | 2016-05-11 | 哈尔滨理工大学 | Method for synthesizing and controlling cerium dioxide micro-nano structure and morphology by hydrothermal process |
| CN109794277A (en) * | 2019-01-30 | 2019-05-24 | 扬州工业职业技术学院 | A kind of ceria/graphite phase carbon nitride composite material and its application in photocatalysis |
| CN110743543A (en) * | 2019-10-25 | 2020-02-04 | 李家宝 | Three-way catalyst |
| CN110743543B (en) * | 2019-10-25 | 2022-12-06 | 苏州松之源环保科技有限公司 | Tail gas purification device containing three-way catalyst |
| CN110918081A (en) * | 2019-12-04 | 2020-03-27 | 吉林省电力科学研究院有限公司 | Plasma cerium oxide catalyst and preparation method thereof |
| CN112467154A (en) * | 2020-12-03 | 2021-03-09 | 福州大学 | Preparation method of cerium oxide loaded nickel-iron catalyst |
| WO2023125890A1 (en) * | 2021-12-30 | 2023-07-06 | 安集微电子科技（上海）股份有限公司 | Method for synthesizing cerium oxide, cerium oxide, and chemical mechanical polishing solution |
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Application publication date: 20130102 |