CN115028185B - Corn cob cerium oxide and preparation method and application thereof - Google Patents
Corn cob cerium oxide and preparation method and application thereof Download PDFInfo
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- CN115028185B CN115028185B CN202210537714.0A CN202210537714A CN115028185B CN 115028185 B CN115028185 B CN 115028185B CN 202210537714 A CN202210537714 A CN 202210537714A CN 115028185 B CN115028185 B CN 115028185B
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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
- 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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- 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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
Abstract
The invention belongs to the technical field of inorganic nano material preparation, and particularly discloses corn cob cerium oxide and a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) Mixing the aqueous solution of the positive trivalent cerium ions with organic base, adding a surfactant, and uniformly mixing to prepare a mixed solution; (2) And (3) reacting the mixed solution at 120-200 ℃ for 16-30 hours, centrifuging after the reaction is finished, removing upper liquid, washing the obtained powder, and drying to obtain the corn cob cerium oxide. The preparation process is simple, and the requirements on production equipment and process conditions are low; the required raw material varieties are few, and the production cost is very low compared with the traditional process. In addition, corn cob cerium oxide is prepared into polishing solution, which is beneficial to improving the removal rate and the surface quality.
Description
Technical Field
The invention belongs to the technical field of inorganic nano material preparation, and particularly relates to a preparation method and application of planar cerium oxide.
Background
Cerium oxide has the advantages of single crystal form, good electrical property and optical property, and the like, and is widely applied. The current application range of the catalyst is expanded from the fields of luminescent materials, glass polishing agents, catalysts, electronic ceramics, ultraviolet absorbers and the like to the modern high-tech fields of automobile exhaust gas purification catalytic materials, high Wen Yangmin materials, pH sensing materials, solid Oxide Fuel Cell (SOFC) electrode materials, electrochemical reaction promoting materials, chemical mechanical polishing (GMP) grinding materials, metal oxidation and corrosion resistant coating materials, additives and the like.
Chemical mechanical polishing technology is a new technology developed in recent years, and this method can truly planarize the entire silicon wafer surface. In the CMP technique, chemical mechanical polishing slurry is one of the key factors, and has a very critical influence on the planarization effect of CMP. The CMP polishing slurries widely used at present mainly include the following three types: siO2 polishing liquid, ceO2 polishing liquid, alO3 polishing liquid, and the like.
Among these oxide polishing solutions, ceO2 has the characteristics of low hardness, less scratches, high polishing speed, high selectivity in shallow trench isolation (STD polishing), and the like.
In recent years, various cerium oxide materials with various shapes such as cubes, octahedrons, spheres, hollow spheres and the like have been synthesized through different methods, the main preparation methods are methods such as magnetron sputtering, electron beam evaporation, pulse laser deposition, hydrothermal chemical deposition, sol-gel and the like, chinese patent CN1532147 proposes a preparation method of nano cerium oxide particles, chinese patent CM948157 proposes a preparation method of hollow spherical nano cerium oxide, chinese patent CN 112499660A proposes a preparation method of octahedral cerium oxide, chinese patent CN 103274441A proposes a preparation method of nano platy cerium oxide, and corn-cob cerium oxide is rarely reported. Therefore, it is of great importance to study how to synthesize corn cob cerium oxide and its application.
Disclosure of Invention
Aiming at the problems, a preparation method and application of corn cob cerium oxide are provided.
The technical scheme adopted by the invention is as follows:
a preparation method of corn cob cerium oxide comprises the following steps:
(1) Mixing the aqueous solution of the positive trivalent cerium ions with organic base, adding a surfactant, and uniformly mixing to prepare a mixed solution;
(2) And (3) reacting the mixed solution at 120-200 ℃ for 16-30 hours, centrifuging after the reaction is finished, removing upper liquid, washing the obtained powder, and drying to obtain the corn cob cerium oxide.
Preferably, the concentration of the positive trivalent cerium ions in the mixed solution is 0.001-0.01mol/L, and the concentration of the organic alkali is 0.05-0.15mol/L.
Preferably, the molar ratio of the positive trivalent cerium ions to the organic base is 1: (5-20).
Preferably, the mole percentage of the surfactant to the positive trivalent cerium ion is 0.5% -1.5%.
Preferably, the organic base is one or more of ethylenediamine, urea, triethanolamine and ammonium citrate.
Preferably, the trivalent cerium ion is one or more of cerium nitrate, cerium chloride, ammonium cerium nitrate and cerium acetate.
Preferably, the surfactant is one or more of polyvinylpyrrolidone, sodium polyacrylate, polyethylene glycol (molecular weight 200-20000) and fatty alcohol-polyoxyethylene ether.
Preferably, the reaction temperature is 150-180 ℃; the reaction time is 20-25 hours.
The synthesized cerium oxide does not need other special treatment, has good dispersibility and polishing activity, and can be used as an abrasive for ILD polishing. It is another aspect of the present invention to provide a cerium oxide polishing liquid comprising cerium oxide particles obtained by the aforementioned preparation method. The preparation of the slurry and the selection of the components may be selected according to conventional techniques in the art, and by way of example, in the examples herein, a formulation of a particular slurry is provided, including cerium oxide particles, a suspending agent, and an acidity regulator. The fixing is as follows: comprises, by weight, 1+ -0.5% corn cob cerium oxide particles, 0.2+ -0.1% polyvinylpyrrolidone, citric acid to adjust pH to 4+ -0.5, and the balance of ultrapure water.
Compared with the prior art, the invention has the following beneficial effects:
1. the corn cob cerium oxide is synthesized by a hydrothermal method in one step, the preparation process is simple, and the requirements on production equipment and process conditions are low; the required raw material varieties are few, and the production cost is very low compared with the traditional process.
2. No template material is needed, no organic solvent is added, no pollution is caused basically, and the environment is protected; the method avoids the processes of more raw materials, complex process, harsh production condition requirements, calcining and washing with organic reagents in the traditional liquid phase method. The process conditions are mild and controllable, the environment is protected, no pollution is caused, and compared with the traditional preparation method, the method has great progress and production value.
3. By controlling the temperature and the reaction time, pure corn cob cerium oxide with controllable particle size can be prepared.
4. The corn cob cerium oxide is prepared into the polishing solution, wherein cerium oxide particles are positioned on the same plane to do rolling friction movement, so that the contact area is increased, and meanwhile, waste generated by polishing can be taken away more quickly through rolling friction, thereby being beneficial to improving the removal rate and the surface quality.
Drawings
FIG. 1 is an SEM image of corn cob ceria of example 1.
FIG. 2 is a SEM image of corn cob ceria of example 2.
FIG. 3 is an SEM image of corn cob ceria of example 3.
Fig. 4 is a SEM image of cerium oxide of comparative example 1.
Fig. 5 is a SEM image of cerium oxide of comparative example 2.
Fig. 6 is a SEM image of cerium oxide of comparative example 3.
FIG. 7 is a roughness measurement diagram of example 1.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but embodiments of the present invention are not limited thereto, and may be performed with reference to conventional techniques for process parameters that are not specifically noted.
The reagents and raw materials used in the invention are the pure grade reagents for the ridge analysis and are commercially available. The polishing solution is prepared by simply and uniformly mixing the components.
Example 1
1. Preparing 0.04mol/L cerium nitrate aqueous solution at room temperature; in addition, aqueous solutions of urea and polyvinylpyrrolidone were prepared at room temperature, respectively, the urea concentration was 5 times that of cerium nitrate, 0.2mol/L, and the polyvinylpyrrolidone concentration was 1% of cerium nitrate, 0.0004mol/L.
2. And (3) respectively taking 60ml of the urea and polyvinylpyrrolidone solution at room temperature, mixing in a beaker, taking 20ml of the cerium nitrate aqueous solution, and slowly dropwise adding the mixture into the mixed solution of urea and polyvinylpyrrolidone under stirring.
3. Transferring the mixed solution obtained in the step 2 into a reaction kettle, reacting for 24 hours at 180 ℃, taking out and centrifuging after the reaction is finished, removing upper liquid, washing powder obtained by centrifuging, and drying to obtain solid, thus obtaining the corn cob cerium oxide. FIG. 1 is an SEM image of the corn-on-cob ceria prepared in this example.
Example 2
1. Preparing 0.05mol/L cerium chloride aqueous solution at room temperature; in addition, ammonium citrate and sodium polyacrylate solution are respectively prepared at room temperature, wherein the concentration of ammonium citrate is 5 times that of cerium chloride, 0.25mol/L, and the concentration of sodium polyacrylate is 1% of positive trivalent cerium ions, 0.0005mol/L.
2. 80ml of each of the ammonium citrate and sodium polyacrylate solution was placed in a beaker at room temperature and mixed, 16ml of the cerium nitrate aqueous solution was taken and slowly added dropwise to the mixed solution of ammonium citrate and sodium polyacrylate with stirring.
3. Transferring the mixed solution obtained in the step 2 into a reaction kettle, reacting for 28 hours at 160 ℃, taking out and centrifuging after the reaction is finished, removing upper-layer liquid, washing powder obtained by centrifuging, and drying to obtain solid, thus obtaining the corn cob cerium oxide. Fig. 2 is an SEM image of the corn-cob ceria prepared in this example.
Example 3
1. Preparing 0.06mol/L ceric ammonium nitrate aqueous solution at room temperature; in addition, ammonium citrate and sodium polyacrylate solution are respectively prepared at room temperature, wherein the ammonium citrate is 5 times of the positive trivalent cerium ion, the concentration of the sodium polyacrylate is 0.3mol/L, and the concentration of the sodium polyacrylate is 1% of the positive trivalent cerium ion, and is 0.0006mol/L.
2. 60ml of each of the ammonium citrate and sodium polyacrylate solution was placed in a beaker at room temperature and mixed, 15ml of the ammonium cerium nitrate aqueous solution was taken and slowly added dropwise to the mixed solution of ammonium citrate and sodium polyacrylate with stirring.
3. Transferring the mixed solution obtained in the step 2 into a reaction kettle, reacting for 26 hours at 150 ℃, taking out and centrifuging after the reaction is finished, removing upper-layer liquid, washing powder obtained by centrifuging, and drying to obtain solid, thus obtaining the corn cob cerium oxide.
Example 4
1. Preparing 0.07mol/L cerium nitrate aqueous solution at room temperature; in addition, ethylenediamine and PEG4000 solutions were prepared at room temperature, respectively, the ethylenediamine concentration was 5 times that of cerium nitrate, 0.35mol/L, and the PEG4000 concentration was 1% of positive trivalent cerium ion, 0.0007mol/L.
2. 80ml of each of the ethylenediamine and PEG4000 solutions was placed in a beaker and mixed at room temperature, 20ml of the aqueous cerium nitrate solution was taken and slowly added dropwise to the mixed solution of ethylenediamine and PEG4000 with stirring.
3. Transferring the mixed solution obtained in the step 2 into a reaction kettle, reacting for 25 hours at 170 ℃, taking out and centrifuging after the reaction is finished, removing upper-layer liquid, washing powder obtained by centrifuging, and drying to obtain solid, thus obtaining the corn cob cerium oxide.
Example 5
1. Preparing 0.08mol/L cerium chloride aqueous solution at room temperature; in addition, urea and PEG6000 solutions are respectively prepared at room temperature, wherein the concentration of urea is 5 times of that of cerium chloride, 0.4mol/L, and the concentration of PEG6000 is 1% of that of positive trivalent cerium ions, and 0.0008mol/L.
2. Placing 60ml of each of the urea and PEG6000 solution into a beaker at room temperature, taking 12ml of the cerium chloride aqueous solution, and slowly dropwise adding the cerium chloride aqueous solution into the mixture of the urea and the PEG6000 solution under stirring;
3. transferring the mixed solution obtained in the step 2 into a reaction kettle, reacting for 18 hours at 200 ℃, taking out and centrifuging after the reaction is finished, removing upper-layer liquid, washing powder obtained by centrifuging, and drying to obtain solid, thus obtaining the corn cob cerium oxide.
Example 6
1. Preparing 0.03mol/L cerium acetate aqueous solution at room temperature; in addition, ethylenediamine and polyvinylpyrrolidone solutions were prepared at room temperature, respectively, the ethylenediamine concentration was 5 times that of cerium acetate, 0.15mol/L, and the polyvinylpyrrolidone concentration was 1% of that of cerium acetate, 0.0003mol/L.
2. 70ml of each of the ethylenediamine and polyvinylpyrrolidone solution is placed in a beaker at room temperature, 14ml of the cerium acetate aqueous solution is taken, and the mixture solution of ethylenediamine and polyvinylpyrrolidone is slowly added dropwise under stirring;
3. transferring the mixed solution obtained in the step 2 into a reaction kettle, reacting for 27 hours at 190 ℃, taking out and centrifuging after the reaction is finished, removing upper-layer liquid, washing powder obtained by centrifuging, and drying to obtain solid, thus obtaining the corn cob cerium oxide.
Example 7
1. Preparing 0.03mol/L cerium acetate aqueous solution at room temperature; in addition, the ethylenediamine and polyethylene glycol 400 solutions are respectively prepared at room temperature, wherein the concentration of ethylenediamine is 5 times that of cerium acetate, 0.15mol/L, and the concentration of polyethylene glycol 400 is 5% that of cerium acetate, 0.0015mol/L.
2. 70ml of each of the ethylenediamine and polyethylene glycol 400 solution is placed in a beaker at room temperature, 14ml of the cerium acetate aqueous solution is taken, and the mixture solution of ethylenediamine and polyethylene glycol 400 is slowly added dropwise under stirring;
3. transferring the mixed solution obtained in the step 2 into a reaction kettle, reacting for 30 hours at 120 ℃, taking out and centrifuging after the reaction is finished, removing upper-layer liquid, washing powder obtained by centrifuging, and drying to obtain solid, thus obtaining the corn cob cerium oxide.
Comparative example 1
The present invention is different from example 1 in that: lack of surfactant
1. Preparing 0.04mol/L cerium nitrate aqueous solution at room temperature; in addition, a urea solution is prepared at room temperature, and the concentration of urea is 5 times that of cerium nitrate and is 0.2mol/L.
2. Placing 60ml of the urea solution into a beaker at room temperature, taking 20ml of the cerium nitrate aqueous solution, and slowly dropwise adding the cerium nitrate aqueous solution into the urea solution under stirring;
3. transferring the mixed solution obtained in the step 2 into a reaction kettle, reacting for 24 hours at 180 ℃, taking out and centrifuging after the reaction is finished, removing upper liquid, washing powder obtained by centrifuging, and drying to obtain solid, so that cerium oxide can be obtained, and a rod shape cannot be formed when a surfactant is absent. Fig. 4 is an SEM image of cerium oxide prepared in this example.
Comparative example 2
The present invention is different from example 1 in that: using strong bases
1. Preparing 0.04mol/L cerium nitrate aqueous solution at room temperature; in addition, potassium hydroxide and polyvinylpyrrolidone solution were prepared at room temperature, the concentration of potassium hydroxide was 5 times that of cerium nitrate, 0.2mol/L, and the concentration of polyvinylpyrrolidone was 1% that of cerium nitrate, 0.0004mol/L.
2. Mixing 60ml of each of the potassium hydroxide and polyvinylpyrrolidone solution in a beaker at room temperature, taking 20ml of the cerium nitrate aqueous solution, and slowly dropwise adding the mixture into the mixed solution of the potassium hydroxide and polyvinylpyrrolidone under stirring;
3. transferring the mixed solution obtained in the step 2 into a reaction kettle, reacting for 24 hours at 180 ℃, taking out and centrifuging after the reaction is finished, removing upper-layer liquid, washing powder obtained by centrifuging, and drying to obtain solid, thus obtaining cerium oxide. Fig. 5 is an SEM image of the cerium oxide produced in this example.
Comparative example 3
The present invention is different from example 1 in that: high surfactant content
1. Preparing 0.04mol/L cerium nitrate aqueous solution at room temperature; in addition, potassium hydroxide and polyvinylpyrrolidone solution were prepared at room temperature, the concentration of potassium hydroxide was 5 times that of cerium nitrate, 0.2mol/L, and the concentration of polyvinylpyrrolidone was 10% that of cerium nitrate, 0.004mol/L.
2. 60ml of each of the potassium hydroxide and polyvinylpyrrolidone solution was placed in a beaker at room temperature, 20ml of the cerium nitrate aqueous solution was taken, and the mixture of potassium hydroxide and polyvinylpyrrolidone solution was slowly added dropwise with stirring.
3. Transferring the mixed solution obtained in the step 2 into a reaction kettle, reacting for 24 hours at 180 ℃, taking out and centrifuging after the reaction is finished, removing upper-layer liquid, washing powder obtained by centrifuging, and drying to obtain solid, thus obtaining cerium oxide. Fig. 6 is an SEM image of the cerium oxide produced in this example.
The above examples and comparative examples were formulated into polishing solutions, and blank wafers were polished under polishing conditionsThe polishing parameters were the same as follows: the DuPont IC1010 polishing pad was pressed down at 3psi using a Hua Haiqing family Universal 300 polisher with turntable speed/polishing head speed = 60/80rpm for 60 seconds with a chemical mechanical polishing slurry flow rate of 200mL/min. Wafer slices for polishing are supplied by Shanghai's electronic technology Co. Silicon oxide film thickness from J.A. Woollam company spectroscopic ellipsometer-And dividing the thickness difference measured before and after polishing by the polishing time to obtain the removal rate of the silicon oxide film, wherein the polishing time is 1 minute.
TABLE 1
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (6)
1. The polishing solution is characterized by taking corn cob cerium oxide particles as an abrasive, wherein the corn cob cerium oxide is prepared by the following steps:
(1) Mixing the aqueous solution of the positive trivalent cerium ions with organic base, adding a surfactant, and uniformly mixing to prepare a mixed solution; the molar ratio of the positive trivalent cerium ions to the organic base is 1: (5-20); the mole percentage of the surfactant and the positive trivalent cerium ion is 0.5% -1.5%;
(2) And (3) reacting the mixed solution at 120-200 ℃ for 16-30 hours, centrifuging after the reaction is finished, removing upper liquid, washing the obtained powder, and drying to obtain the corn cob cerium oxide.
2. The polishing liquid according to claim 1, wherein the concentration of the positive trivalent cerium ions in the mixed liquid is 0.001 to 0.01mol/L, and the concentration of the organic base is 0.05 to 0.15mol/L.
3. The polishing liquid according to claim 1 or 2, wherein the organic base is one or more of ethylenediamine, urea, triethanolamine, and ammonium citrate;
the aqueous solution of the positive trivalent cerium ions is one or more of cerium nitrate aqueous solution, cerium chloride aqueous solution, ammonium cerium nitrate aqueous solution and cerium acetate aqueous solution;
the surfactant is one or more of polyvinylpyrrolidone, sodium polyacrylate, polyethylene glycol and fatty alcohol polyoxyethylene ether.
4. The polishing liquid according to claim 1 or 2, wherein the reaction temperature is 150 to 180 ℃; the reaction time is 20-25 hours.
5. The polishing liquid according to claim 1 or 2, comprising corn cob cerium oxide particles, a suspending agent, and an acidity regulator.
6. The polishing liquid according to claim 5, comprising, in weight percent, 1.+ -. 0.5% of corn cob cerium oxide particles, 0.2.+ -. 0.1% of polyvinylpyrrolidone, citric acid to adjust pH to 4.+ -. 0.5, the balance being ultrapure water.
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| WO2016106765A1 (en) * | 2014-12-29 | 2016-07-07 | 尹先升 | Method for preparing cerium oxide crystals and cmp polishing application thereof |
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| CN111592027A (en) * | 2020-05-29 | 2020-08-28 | 淮阴师范学院 | Preparation method of high specific surface area cerium dioxide |
| WO2021105174A1 (en) * | 2019-11-26 | 2021-06-03 | Rhodia Operations | Cerium based particles, process for producing the same and uses thereof in polishing |
| CN113247941A (en) * | 2021-06-16 | 2021-08-13 | 四川大学 | Method for synthesizing uniform spherical nano cerium oxide material at low temperature |
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2022
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| WO2016106765A1 (en) * | 2014-12-29 | 2016-07-07 | 尹先升 | Method for preparing cerium oxide crystals and cmp polishing application thereof |
| CN107511145A (en) * | 2017-08-11 | 2017-12-26 | 武汉理工大学 | A kind of bar-shaped hierarchical organization pucherite material of corn of nano-particle accumulation and preparation method thereof |
| WO2021105174A1 (en) * | 2019-11-26 | 2021-06-03 | Rhodia Operations | Cerium based particles, process for producing the same and uses thereof in polishing |
| CN111592027A (en) * | 2020-05-29 | 2020-08-28 | 淮阴师范学院 | Preparation method of high specific surface area cerium dioxide |
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