CN115465879A - A kind of preparation method of spherical CeO2 - Google Patents
A kind of preparation method of spherical CeO2 Download PDFInfo
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- CN115465879A CN115465879A CN202110653046.3A CN202110653046A CN115465879A CN 115465879 A CN115465879 A CN 115465879A CN 202110653046 A CN202110653046 A CN 202110653046A CN 115465879 A CN115465879 A CN 115465879A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 title description 6
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 title description 6
- 239000000843 powder Substances 0.000 claims abstract description 11
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims abstract description 10
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 6
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 5
- 150000000703 Cerium Chemical class 0.000 claims abstract description 5
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 235000019253 formic acid Nutrition 0.000 claims abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical group [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 4
- VZTDIZULWFCMLS-UHFFFAOYSA-N ammonium formate Chemical compound [NH4+].[O-]C=O VZTDIZULWFCMLS-UHFFFAOYSA-N 0.000 claims 2
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims 1
- 238000005498 polishing Methods 0.000 abstract description 4
- UADULFIZHZKEOP-UHFFFAOYSA-K cerium(3+);triformate Chemical compound [Ce+3].[O-]C=O.[O-]C=O.[O-]C=O UADULFIZHZKEOP-UHFFFAOYSA-K 0.000 abstract description 3
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- 239000011521 glass Substances 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- -1 sensors Substances 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract 2
- 239000007784 solid electrolyte Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 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
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
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- 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
- C01F17/10—Preparation or treatment, e.g. separation or purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- 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
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
技术领域technical field
本发明属于纳米功能材料制备技领域，具体涉及一种球形CeO2的制备方法。 The invention belongs to the technical field of preparation of nano functional materials, and in particular relates to a preparation method of spherical CeO2.
背景技术Background technique
氧化铈是一种重要的稀土化合物，已广泛应用于固体氧化物燃料电池的抛光粉、催化剂、气体传感器和电极材料等领域。由于纳米材料具有不同于普通材料的独特物理化学性质，因此纳米氧化铈材料的合成受到研究者的广泛关注。且由于CeO2的相应性能与其形貌有密切关联，包括特殊的尺寸和形状等因素，因此控制其形貌的合成已成为调整其性能的重要途径。目前已有许多方法，包括喷雾热解、声化学和微波辅助热分解、电合成、均相沉淀法和水热法等，被成功地用于制备纳米二氧化铈颗粒。近几十年来，各种形貌的CeO2颗粒，包括纳米棒、纳米管、纳米线和纳米片等形貌被逐渐开发出来。然而，采用尺寸可控的球形CeO2颗粒的研究却少有报道。Cerium oxide is an important rare earth compound, which has been widely used in the fields of solid oxide fuel cell polishing powder, catalyst, gas sensor and electrode material. Because nanomaterials have unique physical and chemical properties different from ordinary materials, the synthesis of nanocerium oxide materials has attracted extensive attention of researchers. And because the corresponding properties of CeO 2 are closely related to its morphology, including factors such as special size and shape, controlling the synthesis of its morphology has become an important way to adjust its properties. Many methods, including spray pyrolysis, sonochemical and microwave-assisted pyrolysis, electrosynthesis, homogeneous precipitation, and hydrothermal methods, have been successfully used to prepare nanoceria particles. In recent decades, various morphologies of CeO2 particles, including nanorods, nanotubes, nanowires, and nanosheets, have been gradually developed. However, studies employing size - controllable spherical CeO2 particles are rarely reported.
发明内容Contents of the invention
发明主要是通过以球形甲酸铈为前驱体，所制得的甲酸铈均匀性良好。并通过空气中煅烧得到结晶性良好的球形CeO2。该法简单方便，且易于批量生产。The invention mainly uses spherical cerium formate as a precursor, and the prepared cerium formate has good uniformity. And by calcining in air to obtain spherical CeO 2 with good crystallinity. The method is simple and convenient, and is easy to produce in batches.
本发明的球形CeO2的制备方法，包括如下步骤：Spherical CeO of the present invention The preparation method comprises the steps:
（1）将1mmol可溶性铈盐在20-100mL甲醇中充分混合溶解，得到溶液A。(1) Fully mix and dissolve 1 mmol soluble cerium salt in 20-100 mL methanol to obtain solution A.
（2）将5-10mmol的甲酸或甲酸盐，5-10mmol的二甲胺与5-10mmol表面活性剂PVPK-30在20-100mL甲醇中充分混合溶解，得到溶液B。(2) Fully mix and dissolve 5-10mmol of formic acid or formate, 5-10mmol of dimethylamine and 5-10mmol of surfactant PVPK-30 in 20-100mL of methanol to obtain solution B.
（3）将溶液A快速加入到溶液B。静置12 h，离心得到白色粉末。(3) Quickly add solution A to solution B. After standing for 12 h, the white powder was obtained by centrifugation.
（4）将白色粉末在空气氛围下，400-1000℃下煅烧2-10h，得到淡黄色粉末。本发明的有益效果在于：（1）所制备的CeO2颗粒具有高分散、超细、球形完整度好的特征；（2）所制备的球形CeO2颗粒尺寸均匀，D90≤1μm，粒度分布（D90-D10）/(2D50)<1；（3）所制备的CeO2颗粒适用于高端显示玻璃基板的抛光以及芯片的抛光等应用。(4) Calcining the white powder at 400-1000° C. for 2-10 hours in an air atmosphere to obtain a light yellow powder. The beneficial effects of the present invention are: ( 1 ) the prepared CeO2 particles have the characteristics of high dispersion, ultra-fineness, and good spherical integrity; ( 2 ) the prepared spherical CeO2 particles are uniform in size, D90≤1μm, and the particle size distribution ( D90-D10)/(2D50)<1; (3) The prepared CeO 2 particles are suitable for polishing of high-end display glass substrates and polishing of chips.
附图说明Description of drawings
图1为实施例1所得产物的X射线衍射（XRD）谱图。Fig. 1 is the X-ray diffraction (XRD) spectrogram of the product obtained in Example 1.
图2为实施例1所得产物的扫描电镜（SEM）图。Figure 2 is a scanning electron microscope (SEM) image of the product obtained in Example 1.
具体实施方式detailed description
实施例1Example 1
（1）将0.667mmol硝酸铈在30mL甲醇中充分混合溶解，得到溶液A。(1) Thoroughly mix and dissolve 0.667mmol cerium nitrate in 30mL methanol to obtain solution A.
（2）将5mmol的甲酸，5mmol的二甲胺与1g 表面活性剂PVP K-30，在30mL甲醇中充分混合溶解，得到溶液B。将溶液A快速加入到溶液B。静置12h，离心得到白色粉末。500℃下煅烧3h，得到淡黄色粉末。所得产物的X射线衍射（XRD）谱图见图1，形貌见图2。(2) Mix and dissolve 5mmol of formic acid, 5mmol of dimethylamine and 1g of surfactant PVP K-30 in 30mL of methanol to obtain solution B. Solution A was quickly added to solution B. Let it stand for 12 hours, and centrifuge to obtain a white powder. Calcined at 500°C for 3h to obtain light yellow powder. The X-ray diffraction (XRD) spectrum of the obtained product is shown in Figure 1, and the morphology is shown in Figure 2.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101168447A (en) * | 2007-09-24 | 2008-04-30 | 辽宁师范大学 | A kind of preparation method of three-dimensional cerium oxide |
| CN101804318A (en) * | 2010-04-16 | 2010-08-18 | 北京科技大学 | Preparation of lanthanum doping cerium dioxide porous microspheres and application thereof to Cr<6+> removal |
| CN102942204A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Method for preparing cerium dioxide nanometer powder |
| CN108975391A (en) * | 2018-07-26 | 2018-12-11 | 四川理工学院 | A kind of synthetic method of metal oxide nano microballoon |
| CN109336161A (en) * | 2018-11-12 | 2019-02-15 | 合肥师范学院 | A kind of preparation method of CeO2 nanotube, CeO2 nanotube and application |
| CN111592027A (en) * | 2020-05-29 | 2020-08-28 | 淮阴师范学院 | Preparation method of high specific surface area ceria |
| CN111592029A (en) * | 2020-05-29 | 2020-08-28 | 淮阴师范学院 | Preparation method of rod-shaped silver-plated cerium dioxide |
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2021
- 2021-06-11 CN CN202110653046.3A patent/CN115465879B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101168447A (en) * | 2007-09-24 | 2008-04-30 | 辽宁师范大学 | A kind of preparation method of three-dimensional cerium oxide |
| CN101804318A (en) * | 2010-04-16 | 2010-08-18 | 北京科技大学 | Preparation of lanthanum doping cerium dioxide porous microspheres and application thereof to Cr<6+> removal |
| CN102942204A (en) * | 2012-11-20 | 2013-02-27 | 陕西科技大学 | Method for preparing cerium dioxide nanometer powder |
| CN108975391A (en) * | 2018-07-26 | 2018-12-11 | 四川理工学院 | A kind of synthetic method of metal oxide nano microballoon |
| CN109336161A (en) * | 2018-11-12 | 2019-02-15 | 合肥师范学院 | A kind of preparation method of CeO2 nanotube, CeO2 nanotube and application |
| CN111592027A (en) * | 2020-05-29 | 2020-08-28 | 淮阴师范学院 | Preparation method of high specific surface area ceria |
| CN111592029A (en) * | 2020-05-29 | 2020-08-28 | 淮阴师范学院 | Preparation method of rod-shaped silver-plated cerium dioxide |
Non-Patent Citations (5)
| Title |
|---|
| LIU XIUFANG ET AL.: "Mesoporous-shelled CeO2 hollow nanospheres synthesized by a one-pot hydrothermal route and their catalytric performance", 《CRYSTENGCOMM》, vol. 15, no. 38, pages 7769 - 7775 * |
| LOPEZ-MENA E.R. ET AL.: "Simple Route to Obtain Nanostructured CeO2 Microspheres and CO Gas Sensing performance", 《NANOSCALE RESEARCH LETTERS》, vol. 12, pages 1 - 10, XP021243044, DOI: 10.1186/s11671-017-1951-x * |
| 李汶骏等: "形貌对CeO2纳米颗粒紫外吸收性能的影响", 《硅酸盐通报》, vol. 30, no. 07, pages 1401 - 1404 * |
| 王成云等: "非水溶剂水热法制备CeO2纳米粉", 《化学研究与应用》, no. 04, pages 402 - 405 * |
| 窦正杰;郑育英;方岩雄;: "表面活性剂辅助合成不同形貌纳米CeO_2研究进展", 化工新型材料, no. 09, pages 43 - 45 * |
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