CN114671451A - Synthesis method and use method of cerium oxide - Google Patents
Synthesis method and use method of cerium oxide Download PDFInfo
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- CN114671451A CN114671451A CN202011564786.1A CN202011564786A CN114671451A CN 114671451 A CN114671451 A CN 114671451A CN 202011564786 A CN202011564786 A CN 202011564786A CN 114671451 A CN114671451 A CN 114671451A
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- cerium
- synthesis according
- solution
- cerium oxide
- raw material
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- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 35
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000001308 synthesis method Methods 0.000 title abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000005498 polishing Methods 0.000 claims abstract description 31
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 17
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- 239000002244 precipitate Substances 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 25
- 230000015572 biosynthetic process Effects 0.000 claims description 21
- 238000003786 synthesis reaction Methods 0.000 claims description 21
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 8
- 150000000703 Cerium Chemical class 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- HKVFISRIUUGTIB-UHFFFAOYSA-O azanium;cerium;nitrate Chemical compound [NH4+].[Ce].[O-][N+]([O-])=O HKVFISRIUUGTIB-UHFFFAOYSA-O 0.000 claims description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 2
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 claims description 2
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 10
- 239000012716 precipitator Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- DRVWBEJJZZTIGJ-UHFFFAOYSA-N cerium(3+);oxygen(2-) Chemical class [O-2].[O-2].[O-2].[Ce+3].[Ce+3] DRVWBEJJZZTIGJ-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical group N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
- 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
-
- 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
- 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
-
- 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
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Analytical Chemistry (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
Abstract
The invention provides a synthesis method of cerium oxide, which comprises the steps of adding a cerium source water solution into a precipitator solution to generate a raw material solution; introducing nitrogen into the raw material solution, and fully stirring the raw material solution; filtering the raw material solution to obtain a precipitate; drying the precipitate under the protection of nitrogen; and roasting the precipitate under the protection of nitrogen to obtain the cerium oxide. And a method of using the above cerium oxide for chemical mechanical polishing. The cerium oxide synthesized by the method of the present invention has good CMP polishing activity.
Description
Technical Field
The invention relates to the field of chemical mechanical polishing, in particular to a synthesis method of cerium oxide and a use method thereof.
Background
Cerium oxide is an important polishing abrasive and has wide application in integrated circuit CMP. Can achieve high polishing effect at lower solid content, so that the polishing agent has great attention as an abrasive in the field of chemical mechanical polishing solution. For example, cerium oxide has been widely reported as an abrasive for Shallow Trench Isolation (STI) polishing (e.g., ZL201310495424.5, ZL 200510069987.3). Meanwhile, compared with the polishing solution using the traditional silicon oxide or aluminum oxide material as the abrasive, the chemical mechanical polishing solution using cerium oxide as the abrasive has larger application prospect and market advantage in performance and cost.
Studies have shown that when cerium oxide is used as an abrasive, its own particle characteristics are critical to the polishing effect. As in STI polishing applications, there are reports in the literature that cerium oxide particle size, morphology, and defect generation during polishing and polishing rate selectivity all have significant effects
Meanwhile, the Ce ion valence distribution on the surface of the cerium oxide particles plays a key role in the polishing characteristics. Ce3+And Ce4+The proportion in the cerium oxide particles has an important influence on the polishing activity thereof. The invention synthesizes cerium oxide nano-particles formed by mixing three-valence cerium and four-valence cerium by introducing cerium salts with different valence states as raw materials, thereby realizing the control synthesis of the valence state composition on the surface of the cerium oxide nano-particles. The synthesized cerium oxide is applied to CMP polishing and shows unique CMP polishing characteristics.
Disclosure of Invention
The invention discloses a synthesis method of cerium oxide, which comprises the steps of adding a cerium source water solution into a precipitator solution to generate a raw material solution; introducing nitrogen into the raw material solution, and fully stirring the raw material solution; filtering the raw material solution to obtain a precipitate; drying the precipitate under the protection of nitrogen; and roasting the precipitate under the protection of nitrogen to obtain the cerium oxide.
Preferably, the cerium source contains Ce3+And Ce4+，Ce3+/Ce4+The molar ratio of 1/1-1/1000.
Preferably, the Ce is3+/Ce4+The molar ratio of 1/10-1/100.
Preferably, the molar ratio of the cerium source to the precipitant is (1.0/3.5) - (1.0/6.0).
Preferably, the cerium source is a soluble cerium salt.
Preferably, the soluble cerium salt is one or more of cerium chloride, cerium nitrate, cerium acetate, ammonium cerium nitrate and cerium sulfate.
Preferably, the soluble cerium salt is cerium nitrate and/or ammonium cerium nitrate.
Preferably, the concentration of the cerium source aqueous solution is 0.1M to 1.0M.
Preferably, the concentration of the cerium source aqueous solution is 0.2M to 0.6M.
Preferably, the precipitating agent is a soluble base.
Preferably, the soluble alkali is one or more of sodium hydroxide, potassium hydroxide and ammonia water.
Preferably, the soluble base is ammonia.
Preferably, the concentration of the precipitant solution is 0.1M to 3.0M.
Preferably, the concentration of the precipitant solution is 0.5M to 1.5M.
Preferably, the roasting temperature under the protection of nitrogen is 300-750 ℃.
Preferably, the roasting temperature under the protection of nitrogen is 400-750 ℃.
Preferably, the roasting time is 1.0-8.0 h.
Preferably, the roasting time is 3.0-6.0 h.
The invention also provides a method of using a cerium oxide, using any of the cerium oxides as described above for chemical mechanical polishing.
The cerium oxide synthesized using the cerium oxide synthesis method of the present invention has an excellent polishing effect.
Detailed Description
The advantages of the invention are further illustrated below with reference to specific examples.
The cerium oxides of examples 1 to 7 and comparative examples 1 to 4 were synthesized according to the reactants and their concentrations shown in table 1, and according to the corresponding synthesis conditions. The specific synthesis steps are as follows:
s1: adding a cerium source aqueous solution into a precipitant solution to generate a raw material solution;
s2: introducing nitrogen into the raw material solution, and fully stirring the raw material solution for 30 min;
s3: filtering the raw material solution to obtain a precipitate, wherein the cleaning step has no special requirement, can be solid-liquid separation in a centrifugal mode and realize washing for multiple times to remove liquid-phase impurity ions, and can also be used in a filtering mode, and the cleaning step has little influence on the product, and the invention is not particularly limited herein;
s4: drying the precipitate under the protection of nitrogen at 70-100 deg.C;
s5: and roasting the precipitate under the protection of nitrogen to obtain the cerium oxide.
TABLE 1 kinds, concentrations and synthesis conditions of reactants of examples 1-7 and comparative examples 1-4
After obtaining the cerium oxide solids of examples 1 to 7 and comparative examples 1 to 4, they were subjected to dispersion treatment. And preparing a cerium oxide dispersion. And further preparing cerium oxide dispersion liquid into polishing liquid, respectively preparing aqueous dispersion liquid with 1 wt% solid content and pH of about 4.5, and measuring polishing Removal Rate (RR) of the TEOS blank wafer under different pressure conditions.
The polishing conditions were Mirra, IC1010 pad, Platten and Carrier speeds of 93rpm and 87rpm, respectively, 3psi pressure, 150mL/min slurry flow rate, and 60 seconds polishing time.
TABLE 2 results of experiments for polishing cerium oxide dispersions corresponding to examples 1 to 7 and comparative examples 1 to 4
By comparison, the polishing rate of the cerium oxide of comparative examples 1-2 was lower than that of the cerium oxide particles of examples 1-7, indicating that the single valence cerium source had relatively low polishing activity, and that comparative example 3 indicated that the sample prepared at too low firing temperature had no polishing activity, and that comparative example 4 showed high polishing activity, but the particles were seriously agglomerated and were difficult to disperse, and thus, were not suitable for CMP applications. Whereas the cerium oxides of examples 1 to 7 have higher polishing activity.
It should be noted that the embodiments of the present invention have been described in terms of preferred embodiments, and not by way of limitation, and that those skilled in the art can make modifications and variations of the embodiments described above without departing from the spirit of the invention.
Claims (19)
1. A method for synthesizing cerium oxide is characterized by comprising
Adding a cerium source aqueous solution into a precipitant solution to generate a raw material solution;
introducing nitrogen into the raw material solution, and fully stirring the raw material solution;
filtering the raw material solution to obtain a precipitate;
drying the precipitate under the protection of nitrogen;
and roasting the precipitate under the protection of nitrogen to obtain the cerium oxide.
2. The method of synthesis according to claim 1,
the cerium source contains Ce3+And Ce4+，Ce3+/Ce4+The molar ratio of (A) is 1/1-1/1000.
3. The method of synthesis according to claim 2,
the Ce3+/Ce4+The molar ratio of (A) is 1/10-1/100.
4. The method of synthesis according to claim 1,
the molar ratio of the cerium source to the precipitant is (1.0/3.5) - (1.0/6.0).
5. The method of synthesis according to claim 1,
the cerium source is a soluble cerium salt.
6. The method of synthesis according to claim 5,
the soluble cerium salt is one or more of cerium chloride, cerium nitrate, cerium acetate, ammonium cerium nitrate and cerium sulfate.
7. The method of synthesis according to claim 6,
the soluble cerium salt is cerium nitrate and/or ammonium cerium nitrate.
8. The method of synthesis according to claim 1,
the concentration of the cerium source water solution is 0.1M-1.0M.
9. The method of synthesis according to claim 8,
the concentration of the cerium source water solution is 0.2M-0.6M.
10. The method of synthesis according to claim 1,
the precipitant is soluble alkali.
11. The method of synthesis according to claim 10,
the soluble alkali is one or more of sodium hydroxide, potassium hydroxide and ammonia water.
12. The method of synthesis according to claim 11,
the soluble alkali is ammonia water.
13. The method of synthesis according to claim 1,
the concentration of the precipitant solution is 0.1M-3.0M.
14. The method of synthesis according to claim 13,
the concentration of the precipitant solution is 0.5M-1.5M.
15. The method of synthesis according to claim 1,
the roasting temperature is 300-750 ℃ under the protection of nitrogen.
16. The method of synthesis according to claim 15,
the roasting temperature is 400-750 ℃ under the protection of nitrogen.
17. The method of synthesis according to claim 1,
The roasting time is 1.0-8.0 h.
18. The method of synthesis according to claim 17,
the roasting time is 3.0-6.0 h.
19. A method of using the cerium oxide as claimed in any one of claims 1 to 18 for chemical mechanical polishing.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011564786.1A CN114671451A (en) | 2020-12-25 | 2020-12-25 | Synthesis method and use method of cerium oxide |
| PCT/CN2021/142295 WO2022135608A1 (en) | 2020-12-25 | 2021-12-29 | Synthesis method and use method for cerium oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011564786.1A CN114671451A (en) | 2020-12-25 | 2020-12-25 | Synthesis method and use method of cerium oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114671451A true CN114671451A (en) | 2022-06-28 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011564786.1A Pending CN114671451A (en) | 2020-12-25 | 2020-12-25 | Synthesis method and use method of cerium oxide |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN114671451A (en) |
| WO (1) | WO2022135608A1 (en) |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7368388B2 (en) * | 2005-04-15 | 2008-05-06 | Small Robert J | Cerium oxide abrasives for chemical mechanical polishing |
| FR2906800B1 (en) * | 2006-10-09 | 2008-11-28 | Rhodia Recherches & Tech | LIQUID SUSPENSION AND POWDER OF CERIUM OXIDE PARTICLES, PROCESSES FOR PREPARING THE SAME, AND USE IN POLISHING |
| CN103043700A (en) * | 2013-01-10 | 2013-04-17 | 淄博包钢灵芝稀土高科技股份有限公司 | Method for preparing cerium-oxide polishing powder |
| CN105800664A (en) * | 2014-12-29 | 2016-07-27 | 安集微电子（上海）有限公司 | Method for preparing ceria abrasive and application thereof in CMP (Chemical Mechanical Polishing) |
| CN109761260B (en) * | 2019-03-27 | 2021-10-12 | 淄博加华新材料有限公司 | Rare earth and zirconium doped cerium dioxide and preparation method thereof |
-
2020
- 2020-12-25 CN CN202011564786.1A patent/CN114671451A/en active Pending
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2021
- 2021-12-29 WO PCT/CN2021/142295 patent/WO2022135608A1/en active Application Filing
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| Publication number | Publication date |
|---|---|
| WO2022135608A1 (en) | 2022-06-30 |
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