CN114032034A - CeO for chemical mechanical polishing2Method for producing abrasive particles and use thereof - Google Patents
CeO for chemical mechanical polishing2Method for producing abrasive particles and use thereof Download PDFInfo
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- CN114032034A CN114032034A CN202111511606.8A CN202111511606A CN114032034A CN 114032034 A CN114032034 A CN 114032034A CN 202111511606 A CN202111511606 A CN 202111511606A CN 114032034 A CN114032034 A CN 114032034A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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Abstract
The invention discloses CeO for chemical mechanical polishing2A method of making abrasive particles comprising the steps of: weighing cerium salt and molten salt according to a molar ratio of 1 (5-30), grinding, mixing and drying in a crucible; step two, placing the mixed salt mixed and dried in the step one into a tubular atmosphere furnace, heating to 700-800 ℃ at a heating rate of 1-5 ℃/min, roasting, keeping the temperature for 2-4 h, cooling to room temperature at a rate of 1-5 ℃/min after the heat preservation is finished, washing the reacted product with deionized water to obtain a precipitate, namely CeO2A nanoparticle; CeO prepared by the method2The nanoparticles are configured as CeO2The base chemical mechanical polishing solution is suitable for efficient polishing of silicon oxide products, the preparation method has the characteristics of cheap selected raw materials, simple preparation process and short production period, and the prepared CeO2The particles have the characteristic of high polishing efficiency.
Description
Technical Field
The invention belongs to the technical field of functional materials, and relates to a nano material and a preparation method thereofIn particular to CeO for chemical mechanical polishing2A method for preparing grinding particles and application thereof.
Background
Rare earth abrasive particles are one of the most important applications of rare earth raw materials, since CeO2The grinding particles have appropriate mechanical properties and high chemical activity, and can achieve higher polishing effect under the condition of lower solid content, so that CeO2Abrasives are widely used in chemical mechanical polishing processes of silicon oxide materials. Research on CeO for chemical mechanical polishing2The preparation of the abrasive particles has great value in application prospect and economic benefit.
It has been shown in the study that in CeO2In the polishing application of the grinding particles, the morphology and size characteristics of the grinding particles have great influence on the polishing effect, the cerium oxide particles in the polyhedral morphology can not only improve the mechanical action in the polishing process, but also enhance the chemical activity of the grinding material due to the exposure of specific crystal faces, so that the polishing efficiency is obviously improved while the quality of the polished surface is not influenced. Many researchers are working on CeO2The prior art discloses a method for preparing CeO with the size of about 50nm by a sol-gel method2The method of the nano powder has complex preparation process, long particle synthesis period and difficult particle morphology control after twice calcination, and is not suitable for being used in the polishing process. The prior art also discloses a hydrothermal method for preparing nano CeO2The particle method has higher requirements on preparation conditions, the morphology and the size of the nano particles are easy to change obviously if the technological parameters are not adjusted properly, and the polishing efficiency of the abrasive prepared under the optimized technological conditions is lower. Therefore, CeO with cheap raw materials, simple process and high polishing efficiency is developed2The controllable preparation process of the particles has very important practical significance and economic benefit.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide CeO for chemical mechanical polishing2The preparation method of the grinding particles and the application thereof have the advantages of cheap raw materials, simple preparation process and short production periodIs characterized by the simultaneously prepared CeO2The particles have the characteristic of high polishing efficiency.
In order to achieve the purpose, the invention adopts the following technical scheme:
CeO for chemical mechanical polishing2A method of making abrasive particles comprising the steps of:
weighing cerium salt and molten salt according to a molar ratio of 1 (5-30), grinding, mixing and drying;
step two, placing the mixed salt mixed and dried in the step one into a tubular atmosphere furnace, heating the mixed salt from room temperature to 700-800 ℃ at the heating rate of 1-5 ℃/min, roasting, keeping the temperature for 2-4 h, cooling the mixed salt to 500 ℃ at the speed of 1-5 ℃/min after the heat preservation is finished, naturally cooling the mixed salt to room temperature, and cleaning the reacted product with deionized water to obtain a precipitate, namely CeO2And (3) nanoparticles.
Preferably, the cerium salt is any one of cerium nitrate hexahydrate, cerium ammonium nitrate or cerium carbonate.
Preferably, the molten salt is one or two of sodium chloride, potassium chloride, sodium nitrate, potassium nitrate and lithium chloride.
Preferably, when the binary molten salt is selected, the molar ratio of the two molten salts is 1 (1-2).
Preferably, the grinding, mixing and drying method in the first step is that dry grinding is adopted to grind in a crucible, materials are uniformly mixed in absolute ethyl alcohol by using a magnetic stirrer, and the materials are dried for 3-6 hours in a constant-temperature drying oven at 50-80 ℃.
Preferably, the atmosphere of the tube furnace in the second step is argon-hydrogen mixed gas, hydrogen gas, argon gas or nitrogen gas.
Preferably, the flow rate of the atmosphere in the tube furnace is 60 ml/min.
The invention also provides CeO prepared by the preparation method2The application of the nano-particles comprises the steps of adding deionized water, performing ball milling dispersion, adjusting the pH value to 3-6, adjusting the solid content to 0.2-2 wt%, and preparing CeO2Based on a chemical mechanical polishing solution.
Preferably, the ball milling rotation speed of the ball milling dispersion is 400r/min, and the ball milling time is 3-6 h.
Further, configured CeO2The application of the base chemical mechanical polishing solution in the high-efficiency polishing of silicon oxide products.
Compared with the prior art, the invention has the following technical effects:
the preparation method has the characteristics of cheap selected raw materials, simple preparation process and short production period, and the prepared particles have the characteristic of high polishing efficiency;
atmosphere treated CeO prepared according to the invention2The crystal structure of the particles has more oxygen defects, the microscopic morphology of the particles is polyhedral, and the controllable preparation of the particles with the particle size of 100-300 nm can be realized by adjusting the roasting system;
the polishing solution prepared by the grinding particles prepared by the invention can realize higher removal rate and good surface quality in a polishing process of silicon oxide materials, which is attributed to the fact that the oxygen-rich defect particles prepared by the invention have high surface activity and the polyhedron morphology is helpful for removing materials.
Drawings
FIG. 1 shows CeO prepared under the atmosphere conditions as set forth in the examples2XRD spectrogram of the powder;
FIG. 2 is a diagram showing a nearly spherical CeO obtained in example 12SEM image of nanometer powder;
FIG. 3 is a polyhedral CeO prepared in example 22SEM image of nanometer powder;
FIG. 4 is a diagram showing a nearly spherical CeO obtained in example 32SEM image of nanometer powder;
FIG. 5 shows the nearly spherical CeO obtained in example 42SEM image of nanopowder.
Detailed Description
The present invention will be explained in further detail with reference to examples.
Example 1
CeO for chemical mechanical polishing2The preparation method of the grinding particles comprises the following specific process steps:
1.3026g (3mmol) of cerous nitrate hexahydrate, 1.1183g (15mmol) of potassium chloride and 0.8766g (15mmol) of sodium chloride are weighed respectively and ground in a crucible by a dry method to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and uniformly stirring and mixing by magnetic force; pouring the obtained mixture into a crucible, drying the mixture for 5h at 60 ℃ in a constant-temperature drying oven, then placing the mixture and the crucible together in a tubular atmosphere furnace introduced with argon atmosphere for roasting, wherein the gas flow rate is 60ml/min, the temperature is raised to 700 ℃ at the heating rate of 2 ℃/min for roasting, the temperature is kept for 2h, the temperature is reduced to 500 ℃ at the heating rate of 2 ℃/min, and then the mixture is naturally cooled; washing with deionized water after reaction to obtain white precipitate, and drying for later use.
Example 2
CeO for chemical mechanical polishing2The preparation method of the grinding particles comprises the following specific process steps:
1.3026g (3mmol) of cerous nitrate hexahydrate, 1.1183g (15mmol) of potassium chloride and 0.8766g (15mmol) of sodium chloride are weighed respectively and ground in a crucible by a dry method to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and uniformly stirring and mixing by magnetic force; pouring the obtained mixture into a crucible, drying the mixture for 5h at 60 ℃ in a constant-temperature drying box, then placing the mixture and the crucible together in a tubular atmosphere furnace introduced with argon-hydrogen mixed atmosphere for roasting, wherein the gas flow rate is 60ml/min, the temperature is increased to 750 ℃ at the temperature rise rate of 2 ℃/min, the roasting is carried out, the temperature is kept for 2h, the temperature is reduced to 500 ℃ at the temperature rise rate of 2 ℃/min, and then the mixture is naturally cooled; washing with deionized water after reaction to obtain white precipitate, and drying for later use.
Example 3
CeO for chemical mechanical polishing2The preparation method of the grinding particles comprises the following specific process steps:
1.3026g (3mmol) of cerous nitrate hexahydrate, 1.1183g (15mmol) of potassium chloride and 0.8766g (15mmol) of sodium chloride are weighed respectively and ground in a crucible by a dry method to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and uniformly stirring and mixing by magnetic force; pouring the obtained mixture into a crucible, drying the mixture for 5h at 60 ℃ in a constant-temperature drying box, then placing the mixture and the crucible together in a tubular atmosphere furnace introduced with argon-hydrogen mixed atmosphere for roasting, wherein the gas flow rate is 60ml/min, the temperature is increased to 750 ℃ at the temperature rise rate of 5 ℃/min, the roasting is carried out, the temperature is kept for 3h, the temperature is reduced to 500 ℃ at the temperature rise rate of 2 ℃/min, and then the mixture is naturally cooled; washing with deionized water after reaction to obtain white precipitate, and drying for later use.
Example 4
CeO for chemical mechanical polishing2The preparation method of the grinding particles comprises the following specific process steps:
1.3026g (3mmol) of cerous nitrate hexahydrate, 1.1183g (15mmol) of potassium chloride and 0.8766g (15mmol) of sodium chloride are weighed respectively and ground in a crucible by a dry method to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and uniformly stirring and mixing by magnetic force; pouring the obtained mixture into a crucible, drying the mixture for 5h at 60 ℃ in a constant-temperature drying box, then placing the mixture and the crucible together in a tubular atmosphere furnace introduced with argon-hydrogen mixed atmosphere for roasting, wherein the gas flow rate is 60ml/min, the temperature is increased to 800 ℃ at the temperature rise rate of 5 ℃/min for roasting, the temperature is kept for 3h, the temperature is reduced to 500 ℃ at the temperature rise rate of 2 ℃/min, and then the mixture is naturally cooled; washing with deionized water after reaction to obtain white precipitate, and drying for later use.
Example 5
CeO for chemical mechanical polishing2The preparation method of the grinding particles comprises the following specific process steps:
1.3026g (3mmol) of cerous nitrate hexahydrate, 1.1183g (15mmol) of potassium chloride and 1.7552g (30mmol) of sodium chloride are weighed respectively and ground in a crucible by a dry method to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and uniformly stirring and mixing by magnetic force; pouring the obtained mixture into a crucible, drying the mixture for 6h at 50 ℃ in a constant-temperature drying oven, then placing the mixture and the crucible together in a tubular atmosphere furnace introduced with argon atmosphere for roasting, wherein the gas flow rate is 60ml/min, the temperature is increased to 800 ℃ at the temperature rise rate of 5 ℃/min, roasting and keeping the temperature for 3h, the temperature is reduced to 500 ℃ at the temperature rise rate of 2 ℃/min, and then naturally cooling; washing with deionized water after reaction to obtain white precipitate, and drying for later use.
The cerium oxide prepared in example 5 of the present invention was used as an abrasive, deionized water was added and the pH was adjusted to 3.0 to prepare a polishing solution having an abrasive solid content of 0.2 wt%. The described abrasives used for preparing the polishing solution were ball milled for 3h at 400r/min to achieve good dispersion.
Example 6
ChemistryCeO for mechanical polishing2The preparation method of the grinding particles comprises the following specific process steps:
1.6447g (3mmol) of ammonium ceric nitrate and 0.8766g (15mmol) of sodium chloride are weighed respectively and ground in a crucible by a dry method to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and uniformly stirring and mixing by magnetic force; pouring the obtained mixture into a crucible, drying the mixture for 3h at 80 ℃ in a constant-temperature drying oven, then placing the mixture and the crucible together in a tubular atmosphere furnace introduced with hydrogen atmosphere for roasting, wherein the gas flow rate is 60ml/min, the temperature is raised to 750 ℃ at the heating rate of 1 ℃/min for roasting, the temperature is kept for 2h, the temperature is reduced to 500 ℃ at 1 ℃/min, and then the mixture is naturally cooled; washing with deionized water after reaction to obtain white precipitate, and drying for later use.
The cerium oxide prepared in example 6 of the present invention was used as an abrasive, deionized water was added and the pH was adjusted to 4.0 to prepare a polishing solution having an abrasive solid content of 1 wt%. The described abrasives used for preparing the polishing solution were ball milled for 4h at 400r/min to achieve good dispersion.
Example 7
CeO for chemical mechanical polishing2The preparation method of the grinding particles comprises the following specific process steps:
1.381g (3mmol) of cerium carbonate and 6.7098g (90mmol) of potassium chloride are weighed respectively and ground in a crucible by a dry method to grind the raw materials; pouring the mixture into absolute ethyl alcohol, and uniformly stirring and mixing by magnetic force; pouring the obtained mixture into a crucible, drying the mixture for 3h at 70 ℃ in a constant-temperature drying box, then placing the mixture and the crucible together in a tubular atmosphere furnace introduced with nitrogen atmosphere for roasting, wherein the gas flow rate is 60ml/min, the temperature is increased to 800 ℃ at the heating rate of 3 ℃/min for roasting, the temperature is kept for 4h, the temperature is reduced to 500 ℃ at the temperature of 5 ℃/min, and then the mixture is naturally cooled; washing with deionized water after reaction to obtain white precipitate, and drying for later use.
The cerium oxide prepared in example 6 of the present invention was used as an abrasive, deionized water was added and the pH was adjusted to 5.0 to prepare a polishing solution having an abrasive solid content of 2 wt%. The described abrasives used for preparing the polishing solution were ball milled for 6h at 400r/min to achieve good dispersion.
FIG. 1 shows CeO prepared under the atmosphere conditions as set forth in the examples2XRD spectrogram of the powder shows that pure-phase CeO is successfully prepared2A nanoparticle;
FIG. 2 shows the nearly spherical CeO obtained in example 1 by calcining at 700 deg.C for 2 hours at a temperature-rise rate of 2 deg.C/min in the presence of argon as the calcining atmosphere2SEM image of nanometer powder; as shown in the figure, the particle size is 100nm, and the particles are uniformly dispersed.
FIG. 3 is a graph showing the polyhedral CeO prepared in example 2 by calcining at 750 ℃ for 2 hours at a temperature increase rate of 2 ℃/min in the presence of an argon-hydrogen mixture gas as a calcining atmosphere2SEM image of nanometer powder; as shown in FIG. 3, the particle size was 200nm and the particles were uniformly dispersed.
FIG. 4 is a graph showing the nearly spherical CeO obtained in example 3 after baking at 750 ℃ for 3 hours at a temperature rise rate of 5 ℃/min in the presence of an argon-hydrogen mixture gas as a baking atmosphere2SEM image of nanometer powder; as shown in FIG. 4, the particle size was 200nm and the particles were uniformly dispersed.
FIG. 5 shows the nearly spherical CeO obtained in example 4 by baking at 800 ℃ for 3 hours at a temperature rise rate of 5 ℃/min in an argon-hydrogen mixture as a baking atmosphere2SEM image of nanometer powder; as shown in FIG. 5, the particle size was 200nm and the particles were uniformly dispersed.
The cerium oxide prepared in examples 1 to 4 of the present invention was used as an abrasive, deionized water was added and pH was adjusted to 6.0 to prepare a polishing solution having an abrasive solid content of 0.5 wt%. The described abrasives used for preparing the polishing solution were ball milled for 5h at 400r/min to achieve good dispersion. The material removal rate of the polishing solution prepared in the above example was measured.
The polishing solutions prepared in the above embodiments are respectively used to perform chemical mechanical polishing on quartz glass, and in order to ensure the comparability of polishing results, the polishing conditions are set to be the same, and specifically set as follows: the rotating speed of the polishing disc is 80r/min, the rotating speed of the polishing head is 80r/min, the down pressure of the polishing head is 3.5kg, and the polishing time is 3 min. The quartz glass to be polished was a commercial glass (density: 2.2 g/cm)3) The material removal rate is characterized by the ratio of the mass change before and after polishing to the material density, area and time.
Table 1 shows polishing solutions prepared in examples 1 to 4Corresponding to the polishing results, the polishing results of examples show that the prepared CeO2The nano-particles have good polishing performance on quartz glass, namely high polishing rate and low surface roughness. It is necessary to note that the CeO prepared by the claims of the present invention2The particles are suitable for various silicon oxide products (such as quartz glass, K-9 glass, thermal oxidation wafers and the like).
TABLE 1
The above specific examples are merely selected examples to clearly illustrate the effects achieved by the present invention and are not to be construed as simply all embodiments of the present invention. Other variations on the above description of the solution are possible for the practitioner and are not intended to be exhaustive. Any numerical changes that come within the meaning and range of equivalency of the claims are to be embraced within their scope.
Claims (10)
1. CeO for chemical mechanical polishing2A method of making abrasive particles, comprising the steps of:
weighing cerium salt and molten salt according to a molar ratio of 1 (5-30), grinding, mixing and drying;
step two, placing the mixed salt mixed and dried in the step one into a tubular atmosphere furnace, heating the mixed salt from room temperature to 700-800 ℃ at the heating rate of 1-5 ℃/min, roasting, keeping the temperature for 2-4 h, cooling the mixed salt to 500 ℃ at the speed of 1-5 ℃/min after the heat preservation is finished, naturally cooling the mixed salt to room temperature, and cleaning the reacted product with deionized water to obtain a precipitate, namely CeO2And (3) nanoparticles.
2. CeO for chemical mechanical polishing according to claim 12The method for producing abrasive particles is characterized in that the cerium salt is any one of cerium nitrate hexahydrate, cerium ammonium nitrate or cerium carbonate.
3. CeO for chemical mechanical polishing according to claim 12The preparation method of the grinding particles is characterized in that the molten salt is one or two of sodium chloride, potassium chloride, sodium nitrate, potassium nitrate and lithium chloride.
4. CeO for chemical mechanical polishing according to claim 32The preparation method of the grinding particles is characterized in that when binary molten salt is selected, the molar ratio of the two molten salts is 1 (1-2).
5. CeO for chemical mechanical polishing according to claim 12The preparation method of the grinding particles is characterized in that the grinding, mixing and drying method in the first step is that dry grinding is adopted to grind in a crucible, materials are uniformly mixed in absolute ethyl alcohol by a magnetic stirrer, and the materials are dried for 3-6 hours in a constant-temperature drying oven at the temperature of 50-80 ℃.
6. CeO for chemical mechanical polishing according to claim 12The preparation method of the grinding particles is characterized in that the atmosphere of the tubular furnace in the step two is argon-hydrogen mixed gas, hydrogen, argon or nitrogen.
7. CeO for chemical mechanical polishing according to claim 62The preparation method of the grinding particles is characterized in that the introduction flow rate of the atmosphere of the tube furnace is 60 ml/min.
8. CeO prepared by the preparation method of any one of claims 1 to 72The application of the nano-particles is characterized in that deionized water is added, ball milling and dispersing are carried out, the pH range is adjusted to 3-6, the solid content is adjusted to 0.2-2 wt%, and CeO is prepared2Based on a chemical mechanical polishing solution.
9. The CeO of claim 82The application of the nano particles is characterized in that the ball milling rotation speed of ball milling dispersion is 400r/min, and the ball milling time is 3-6 h.
10. The CeO of claim 8 or 92Use of nanoparticles, characterised in that the CeO is present2The application of the base chemical mechanical polishing solution in the high-efficiency polishing of silicon oxide products.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114735743A (en) * | 2022-05-19 | 2022-07-12 | 陕西科技大学 | CeO with polyhedral morphology2Granules and process for their preparation |
| CN116002744A (en) * | 2022-12-19 | 2023-04-25 | 陕西科技大学 | High-activity cerium oxide-based nano abrasive particles, and preparation method and application thereof |
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2021
- 2021-12-06 CN CN202111511606.8A patent/CN114032034A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114735743A (en) * | 2022-05-19 | 2022-07-12 | 陕西科技大学 | CeO with polyhedral morphology2Granules and process for their preparation |
| CN116002744A (en) * | 2022-12-19 | 2023-04-25 | 陕西科技大学 | High-activity cerium oxide-based nano abrasive particles, and preparation method and application thereof |
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