CN116262628A - Method for synthesizing cerium oxide and chemical mechanical polishing solution - Google Patents
Method for synthesizing cerium oxide and chemical mechanical polishing solution Download PDFInfo
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- CN116262628A CN116262628A CN202111524966.1A CN202111524966A CN116262628A CN 116262628 A CN116262628 A CN 116262628A CN 202111524966 A CN202111524966 A CN 202111524966A CN 116262628 A CN116262628 A CN 116262628A
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- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 58
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000005498 polishing Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 20
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 20
- 239000000126 substance Substances 0.000 title claims description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 134
- 238000006243 chemical reaction Methods 0.000 claims abstract description 81
- 239000002244 precipitate Substances 0.000 claims abstract description 48
- 238000001556 precipitation Methods 0.000 claims abstract description 46
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 25
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims abstract description 21
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 19
- 239000000047 product Substances 0.000 claims abstract description 6
- 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 144
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 30
- 239000001099 ammonium carbonate Substances 0.000 claims description 30
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 26
- 238000001816 cooling Methods 0.000 claims description 16
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 12
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 6
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 4
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 4
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 4
- 235000011181 potassium carbonates Nutrition 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 23
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 description 12
- 239000002105 nanoparticle Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000007517 polishing process Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 239000003082 abrasive agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid 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
-
- 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
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a method for synthesizing cerium oxide, which comprises the following steps: s1: preparing a reaction solution: preparing cerium source aqueous solution and precipitant aqueous solution; s2: precipitation reaction: adding the aqueous solution of the precipitant into the aqueous solution of the cerium source, uniformly stirring, and carrying out a precipitation reaction for 2.0-8.0 hours; s3: high-temperature roasting: filtering the precipitate, washing and drying, and roasting the precipitate at high temperature to obtain the cerium oxide product. The method for synthesizing cerium oxide can prepare cerium oxide particles with uniform particle size and narrow particle size distribution, has excellent polishing performance and has wide popularization and application values.
Description
Technical Field
The invention relates to the field of chemical mechanical polishing, in particular to a method for synthesizing cerium oxide and chemical mechanical polishing solution.
Background
The nano cerium oxide is one of important abrasive materials adopted in the chemical mechanical polishing process, and has irreplaceable application characteristics in the polishing processes of an advanced semiconductor system Cheng Jiangou groove isolation, a three-dimensional flash memory, an interlayer dielectric and the like. The grain size distribution and the morphological characteristics of the nano cerium oxide particles have direct influence on the polishing performance. Cerium carbonate is used as a precursor for roasting and synthesizing cerium oxide, and the morphology and the particle size of cerium oxide particles can be controlled and synthesized by controlling the morphology and the particle size of cerium carbonate.
The invention provides a method for controllably synthesizing cerium oxide nano particles, which comprises the steps of controllably synthesizing cerium carbonate nano particles with different particle diameters, washing, drying and roasting at high temperature, then converting into cerium oxide nano particles with corresponding sizes, and dispersing the obtained cerium oxide, so that the cerium oxide can be applied to chemical mechanical polishing.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a method for synthesizing cerium oxide, which comprises the following steps:
s1: preparing a reaction solution: preparing cerium source aqueous solution and precipitant aqueous solution;
s2: precipitation reaction: adding the aqueous solution of the precipitant into the aqueous solution of the cerium source, uniformly stirring, and carrying out a precipitation reaction for 2.0-8.0 hours;
s3: filtering the precipitate, washing and drying, and roasting the precipitate at high temperature to obtain the cerium oxide product.
Preferably, the cerium source is selected from cerium nitrate or cerium chloride; the precipitant is one or more selected from ammonium carbonate, ammonium bicarbonate and potassium carbonate.
Preferably, the cerium source is cerium nitrate; the precipitant is ammonium carbonate.
Preferably, the molar ratio of the cerium source aqueous solution to the precipitant aqueous solution is (1.0/1.0) to (1.0/4.0).
Preferably, the molar concentration of the cerium source aqueous solution is 0.1-1.0M; the molar concentration of the aqueous solution of the precipitant is 0.2-2.0M.
Preferably, the molar concentration of the cerium source aqueous solution is 0.3M; the molar concentration of the aqueous solution of the precipitant is 0.45-0.6M.
Preferably, S2: precipitation reaction: preheating the cerium source aqueous solution to 60-120 ℃, then adding the precipitant aqueous solution into the cerium source aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out the precipitation reaction for 2.0-8.0 hours.
Preferably, S2: precipitation reaction: preheating 1L of the cerium source aqueous solution to 80-95 ℃, then adding 1L of the precipitant aqueous solution into the cerium source aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out the precipitation reaction for 4.0-6.0 hours.
Preferably, S3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying, and roasting the precipitate at 300-800 ℃ for 2.0-6.0 hours to obtain a cerium oxide product.
In another aspect of the present invention, there is also provided a chemical mechanical polishing liquid comprising cerium oxide as described above.
According to the method for synthesizing cerium oxide, cerium carbonate nano particles with uniform particle size distribution are synthesized by controlling the mole ratio of a precipitator to a cerium source, and the cerium oxide nano particles with uniform particle size distribution can be obtained through high-temperature roasting. The cerium oxide particles obtained by the preparation method disclosed by the invention are uniform in particle size distribution, easy to disperse and good in polishing application performance.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of cerium carbonate synthesized by the precipitation reaction in example 1A of the present invention;
FIG. 2 is a Scanning Electron Microscope (SEM) image of cerium carbonate synthesized by the precipitation reaction in example 2 of the present invention;
FIG. 3 is a Scanning Electron Microscope (SEM) image of the cerium oxide synthesized in example 2 of the present invention.
Detailed Description
Advantages of the invention are further described in connection with the following drawings and detailed description.
Example 1A:
s1: preparing a reaction solution: preparing a cerium nitrate aqueous solution and an ammonium carbonate aqueous solution, wherein the molar concentration of the cerium nitrate aqueous solution is 0.3M, and the molar concentration of the ammonium carbonate aqueous solution is 1.2M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 95 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 6.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying, and roasting the precipitate at 300 ℃ for 6.0 hours to obtain cerium oxide 1A.
Example 1B:
s1: preparing a reaction solution: preparing a cerium nitrate aqueous solution and an ammonium carbonate aqueous solution, wherein the molar concentration of the cerium nitrate aqueous solution is 0.3M, and the molar concentration of the ammonium carbonate aqueous solution is 1.2M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 95 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 6.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying, and roasting the precipitate at 500 ℃ for 6.0 hours to obtain cerium oxide 1B.
Example 1C:
s1: preparing a reaction solution: preparing a cerium nitrate aqueous solution and an ammonium carbonate aqueous solution, wherein the molar concentration of the cerium nitrate aqueous solution is 0.3M, and the molar concentration of the ammonium carbonate aqueous solution is 1.2M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 95 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 6.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying, and roasting the precipitate at 800 ℃ for 6.0 hours to obtain cerium oxide 1C.
Example 1D:
s1: preparing a reaction solution: preparing a cerium nitrate aqueous solution and an ammonium carbonate aqueous solution, wherein the molar concentration of the cerium nitrate aqueous solution is 0.3M, and the molar concentration of the ammonium carbonate aqueous solution is 1.2M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 95 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 6.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying, and roasting the precipitate at 800 ℃ for 4.0 hours to obtain cerium oxide 1D.
Example 1E:
s1: preparing a reaction solution: preparing a cerium nitrate aqueous solution and an ammonium carbonate aqueous solution, wherein the molar concentration of the cerium nitrate aqueous solution is 0.3M, and the molar concentration of the ammonium carbonate aqueous solution is 1.2M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 95 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 6.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying, and roasting the precipitate at 800 ℃ for 2.0 hours to obtain cerium oxide 1E.
Example 2:
s1: preparing a reaction solution: preparing a cerium nitrate aqueous solution and an ammonium carbonate aqueous solution, wherein the molar concentration of the cerium nitrate aqueous solution is 0.3M, and the molar concentration of the ammonium carbonate aqueous solution is 0.6M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 95 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 6.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying, and roasting the precipitate at 800 ℃ for 4.0 hours to obtain cerium oxide 2.
Example 3:
s1: preparing a reaction solution: preparing a cerium nitrate aqueous solution and an ammonium carbonate aqueous solution, wherein the molar concentration of the cerium nitrate aqueous solution is 0.3M, and the molar concentration of the ammonium carbonate aqueous solution is 0.51M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 95 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 6.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying, and roasting the precipitate at 800 ℃ for 4.0 hours to obtain cerium oxide 3.
Example 4:
s1: preparing a reaction solution: preparing a cerium nitrate aqueous solution and an ammonium carbonate aqueous solution, wherein the molar concentration of the cerium nitrate aqueous solution is 0.3M, and the molar concentration of the ammonium carbonate aqueous solution is 0.45M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 95 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 4.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying, and roasting the precipitate at 800 ℃ for 4.0 hours to obtain cerium oxide 4.
Example 5:
s1: preparing a reaction solution: preparing a cerium nitrate aqueous solution and an ammonium carbonate aqueous solution, wherein the molar concentration of the cerium nitrate aqueous solution is 0.3M, and the molar concentration of the ammonium carbonate aqueous solution is 0.6M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 80 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 6.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying.
Example 6:
s1: preparing a reaction solution: preparing a cerium nitrate aqueous solution and an ammonium carbonate aqueous solution, wherein the molar concentration of the cerium nitrate aqueous solution is 0.1M, and the molar concentration of the ammonium carbonate aqueous solution is 0.2M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 60 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 8.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying.
Example 7:
s1: preparing a reaction solution: preparing a cerium nitrate aqueous solution and an ammonium carbonate aqueous solution, wherein the molar concentration of the cerium nitrate aqueous solution is 1.0M, and the molar concentration of the ammonium carbonate aqueous solution is 2.0M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 120 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 2.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying.
Example 8:
s1: preparing a reaction solution: preparing a cerium nitrate aqueous solution and a potassium carbonate aqueous solution, wherein the molar concentration of the cerium nitrate aqueous solution is 0.3M, and the molar concentration of the potassium carbonate aqueous solution is 0.6M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 95 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 6.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying.
Example 9:
s1: preparing a reaction solution: preparing a cerium nitrate aqueous solution and an ammonium bicarbonate aqueous solution, wherein the molar concentration of the cerium nitrate aqueous solution is 0.3M, and the molar concentration of the ammonium bicarbonate aqueous solution is 0.6M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 95 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 6.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying.
Example 10:
s1: preparing a reaction solution: preparing a cerium chloride aqueous solution and a potassium carbonate aqueous solution, wherein the molar concentration of the cerium chloride aqueous solution is 0.3M, and the molar concentration of the potassium carbonate aqueous solution is 0.6M;
s2: precipitation reaction: preheating 1L of cerium nitrate aqueous solution to 95 ℃, then adding 1L of cerium nitrate aqueous solution into the cerium nitrate aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out precipitation reaction for 6.0 hours;
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying.
The arrangement of the synthesis conditions of examples 1 to 10 in the present invention is shown in Table 1.
TABLE 1 Synthesis conditions for Synthesis of cerium oxide in examples 1 to 10
Fig. 1, 2 and 3 are SEM images of the products according to the preparation method of examples 1A and 2, respectively, of the present invention: FIG. 1 is an SEM image of cerium carbonate obtained after the precipitation reaction of example 1A, in which the cerium carbonate has a large particle size and poor uniformity; FIG. 2 is an SEM image of cerium carbonate obtained after a precipitation reaction, and it can be observed that cerium carbonate has uniform particles, a size of about 200 nm, and good dispersibility, and no agglomeration phenomenon; fig. 3 is an SEM image of cerium oxide particles obtained by high-temperature roasting of cerium carbonate particles, wherein the cerium oxide particles have a relatively uniform particle size distribution and no obvious agglomeration phenomenon.
The cerium carbonate prepared in examples 3 and 4 had particle sizes of 150 nm and 100 nm, respectively, and remained the original morphology and size after high-temperature calcination to obtain cerium oxide. Therefore, cerium oxide particles with different sizes, which are prepared by the method for synthesizing cerium oxide, have good uniform particle size distribution and better dispersivity.
In order to characterize the polishing performance of the above-mentioned cerium oxide particles, a chemical mechanical polishing liquid containing the cerium oxide was further prepared, and the polishing rate of the polishing liquid to TEOS was further measured. The specific test conditions are as follows:
the cerium oxide powder was prepared as an aqueous dispersion having a solid content of 1wt% and a pH of about 4.5, and polishing Removal Rates (RR) of TEOS blank wafers were measured under different pressure conditions.
The polishing conditions were Mirra, IC1010 polishing pad, platten and Carrier speeds of 93rpm and 87rpm, respectively, a pressure of 3psi, a polishing liquid flow rate of 150mL/min, and a polishing time of 60 seconds.
The measured polishing rates are shown in Table 2.
TABLE 2 polishing Rate of cerium oxide Dispersion of examples 1-10
From the above experimental results, it is understood that the cerium oxide obtained was poor in crystallinity due to the low firing temperature of examples 1A and 1B, resulting in poor polishing performance. After the roasting temperature is increased to 800 ℃, the crystallinity of the prepared cerium oxide is improved, and the polishing performance is also improved. Among them, the cerium oxide prepared in example 2 had a size of about 200 nm, and the polishing effect was optimal. Compared with the existing cerium oxide polishing solution, the cerium oxide particles prepared by the method are approximately spherical in shape and uniform in size, and the wafer is not scratched in the polishing process.
It should be noted that the embodiments of the present invention are preferred and not limited in any way, and any person skilled in the art may make use of the above-disclosed technical content to change or modify the same into equivalent effective embodiments without departing from the technical scope of the present invention, and any modification or equivalent change and modification of the above-described embodiments according to the technical substance of the present invention still falls within the scope of the technical scope of the present invention.
Claims (10)
1. A method for synthesizing cerium oxide is characterized in that,
s1: preparing a reaction solution: preparing cerium source aqueous solution and precipitant aqueous solution;
s2: precipitation reaction: adding the aqueous solution of the precipitant into the aqueous solution of the cerium source, uniformly stirring, and carrying out a precipitation reaction for 2.0-8.0 hours;
s3: high-temperature roasting: filtering the precipitate, washing and drying, and roasting the precipitate at high temperature to obtain the cerium oxide product.
2. The method for synthesizing cerium oxide according to claim 1,
the cerium source is selected from cerium nitrate or cerium chloride;
the precipitant is one or more selected from ammonium carbonate, ammonium bicarbonate and potassium carbonate.
3. The method for synthesizing cerium oxide according to claim 2, wherein,
the cerium source is cerium nitrate;
the precipitant is ammonium carbonate.
4. The method for synthesizing cerium oxide according to claim 1,
the molar ratio of the cerium source aqueous solution to the precipitant aqueous solution is (1.0/1.0) to (1.0/4.0).
5. The method for synthesizing cerium oxide according to claim 1,
the molar concentration of the cerium source aqueous solution is 0.1-1.0M;
the molar concentration of the aqueous solution of the precipitant is 0.2-2.0M.
6. The method for synthesizing cerium oxide according to claim 5,
the molar concentration of the cerium source aqueous solution is 0.3M;
the molar concentration of the aqueous solution of the precipitant is 0.45-0.6M.
7. The method for synthesizing cerium oxide according to claim 1,
s2: precipitation reaction: preheating the cerium source aqueous solution to 60-120 ℃, then adding the precipitant aqueous solution into the cerium source aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out the precipitation reaction for 2.0-8.0 hours.
8. The method for synthesizing cerium oxide according to claim 7,
s2: precipitation reaction: preheating 1L of the cerium source aqueous solution to 80-95 ℃, then adding 1L of the precipitant aqueous solution into the cerium source aqueous solution, uniformly stirring, maintaining the reaction temperature, and carrying out the precipitation reaction for 4.0-6.0 hours.
9. The method for synthesizing cerium oxide according to claim 1,
s3: high-temperature roasting: filtering the precipitate, naturally cooling the precipitate to room temperature, washing and drying, and roasting the precipitate at 300-800 ℃ for 2.0-6.0 hours to obtain a cerium oxide product.
10. A chemical mechanical polishing solution is characterized in that,
comprising cerium oxide obtainable by the process according to any one of claims 1 to 9.
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| JP2004083350A (en) * | 2002-08-28 | 2004-03-18 | Nippon Denko Kk | Method for manufacturing rare earth oxide fine powder having 100 nm or less primary particle size, and rare earth oxide fine powder |
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| WO2023109515A1 (en) | 2023-06-22 |
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