CN116873967A - Preparation method of cerium-yttrium grinding material for CMP - Google Patents
Preparation method of cerium-yttrium grinding material for CMP Download PDFInfo
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- CN116873967A CN116873967A CN202310236021.2A CN202310236021A CN116873967A CN 116873967 A CN116873967 A CN 116873967A CN 202310236021 A CN202310236021 A CN 202310236021A CN 116873967 A CN116873967 A CN 116873967A
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- Prior art keywords
- cerium
- yttrium
- oxide
- cmp
- hydroxide
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- LENJPRSQISBMDN-UHFFFAOYSA-N [Y].[Ce] Chemical compound [Y].[Ce] LENJPRSQISBMDN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000000463 material Substances 0.000 title claims abstract description 29
- 238000000227 grinding Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 56
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical class [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000005498 polishing Methods 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 26
- HXYSINKNCIMABO-UHFFFAOYSA-H [OH-].[Y+3].[Ce+3].[OH-].[OH-].[OH-].[OH-].[OH-] Chemical compound [OH-].[Y+3].[Ce+3].[OH-].[OH-].[OH-].[OH-].[OH-] HXYSINKNCIMABO-UHFFFAOYSA-H 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 229910052727 yttrium Chemical class 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical class [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000012065 filter cake Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 238000000975 co-precipitation Methods 0.000 claims abstract description 10
- 239000002002 slurry Substances 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 6
- 239000000376 reactant Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 38
- 239000003082 abrasive agent Substances 0.000 claims description 16
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 16
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 16
- 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 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 12
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 10
- 239000004202 carbamide Substances 0.000 claims description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 238000001556 precipitation Methods 0.000 claims description 9
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims description 9
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- 239000003945 anionic surfactant Substances 0.000 claims description 7
- 239000002736 nonionic surfactant Substances 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- 239000004094 surface-active agent Substances 0.000 claims description 7
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims description 6
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 6
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N nitrate group Chemical group [N+](=O)([O-])[O-] NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 229920000058 polyacrylate Polymers 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-K Citrate Chemical compound [O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O KRKNYBCHXYNGOX-UHFFFAOYSA-K 0.000 claims description 3
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 238000005054 agglomeration Methods 0.000 claims description 3
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- RZHBMYQXKIDANM-UHFFFAOYSA-N dioctyl butanedioate;sodium Chemical compound [Na].CCCCCCCCOC(=O)CCC(=O)OCCCCCCCC RZHBMYQXKIDANM-UHFFFAOYSA-N 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 3
- 239000012716 precipitator Substances 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 3
- GGHPAKFFUZUEKL-UHFFFAOYSA-M sodium;hexadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCOS([O-])(=O)=O GGHPAKFFUZUEKL-UHFFFAOYSA-M 0.000 claims description 3
- NWZBFJYXRGSRGD-UHFFFAOYSA-M sodium;octadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOS([O-])(=O)=O NWZBFJYXRGSRGD-UHFFFAOYSA-M 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 13
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- 229910001415 sodium ion Inorganic materials 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- 239000000126 substance Substances 0.000 description 10
- 235000012431 wafers Nutrition 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 8
- 229910021641 deionized water Inorganic materials 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- UNJPQTDTZAKTFK-UHFFFAOYSA-K cerium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Ce+3] UNJPQTDTZAKTFK-UHFFFAOYSA-K 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000011229 interlayer Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 4
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 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 3
- 238000009826 distribution Methods 0.000 description 3
- 238000002955 isolation Methods 0.000 description 3
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 3
- 229920005591 polysilicon Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- 239000012695 Ce precursor Substances 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- VLOFLNGRXXADOF-UHFFFAOYSA-N cerium(3+) oxygen(2-) yttrium(3+) Chemical compound [Y+3].[O-2].[Ce+3].[O-2].[O-2] VLOFLNGRXXADOF-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910003849 O-Si Inorganic materials 0.000 description 1
- 229910003872 O—Si Inorganic materials 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-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
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical group O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- DPUCLPLBKVSJIB-UHFFFAOYSA-N cerium;tetrahydrate Chemical compound O.O.O.O.[Ce] DPUCLPLBKVSJIB-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005216 hydrothermal crystallization Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- -1 yttrium ions Chemical class 0.000 description 1
Classifications
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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
- C01F17/218—Yttrium 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
- 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
-
- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a preparation method of a cerium yttrium grinding material for CMP, which comprises the following steps: respectively dissolving soluble salts of cerium and yttrium, mixing to obtain yttrium-cerium mixed solution, and preparing cerium-yttrium hydroxide by adopting a homogeneous coprecipitation method; oxidizing low valence cerium in cerium yttrium hydroxide into high valence cerium, filtering reactants, putting a filter cake into a high pressure reaction kettle, and performing hydrothermal reaction to obtain oxides of cerium and yttrium serving as cerium yttrium grinding materials. The cerium-yttrium polishing slurry prepared by the invention has high purity, the content of metal sodium ions is less than 0.5ppm, the dispersibility is good, the particles are uniform, and the grinding efficiency is high.
Description
This patent application is application number: 202010835590.5, filing date: 8 months and 19 days 2020, name: cerium yttrium abrasive material for CMP and a preparation method thereof.
Technical Field
The invention belongs to the field of rare earth grinding and polishing materials, and particularly relates to a preparation method of a cerium-yttrium grinding material for CMP.
Background
CMP chemical mechanical polishing (Chemical Mechanical Planarization) technology is an indispensable process step in the fabrication of large scale integrated circuits. Is widely used for planarization of inter-layer dielectric (inter-layer dielectric), shallow trench isolation (shallow trench isolation), polysilicon, metal, damascene (dual damascence), and the like. The polishing material is an indispensable consumable material in the process of CMP (chemical mechanical polishing), and CMP is mainly applied to monocrystalline silicon wafer polishing and dielectric layer polishing in integrated circuits, and integrated circuit manufacturing needs to perform a series of physical and chemical operations on monocrystalline silicon wafers, so that the production process is very complex, and CMP technology is repeatedly used in the process of monocrystalline silicon wafer manufacturing and first half manufacturing processes in the complex process.
In the manufacturing link of monocrystalline silicon wafers, the monocrystalline silicon wafers are firstly thinned through chemical corrosion, the roughness is 10-20 mu m at the moment, and the roughness can be controlled within dozens of nm when the steps of rough polishing, fine polishing and the like are carried out. Generally, monocrystalline silicon wafers require more than 2 polishes to achieve a surface that meets the requirements of an integrated circuit.
Because the IC component adopts multilayer three-dimensional wiring, each layer to be etched has very high global flatness so as to ensure global planarization of each layer. Links used in the CMP planarization process include: rugged insulators, conductors, interlayer dielectrics (ILD), damascene metals (e.g., al, cu), shallow Trench Isolation (STI), silicon oxide, polysilicon, etc. in interconnect structures.
With the continuous progress of integrated circuit chip process technology, the demand for CMP process is increasing. CMP technology was first used in silicon oxide polishing to perform global planarization of interlayer dielectric (ILD), and CMP is more widely used in planarization processes of metal tungsten, copper, polysilicon, etc., after an integrated circuit chip enters a 0.35 μm node. As the number of metal wiring layers increases, more steps are required to perform CMP polishing. Taking a 28nm node process as an example, the required CMP times are 12-13 times, and after entering a 7nm process node, the CMP times are doubled to 30-50 times.
Based on SEMI statistics, the global CMP polishing material market size in 2016 reaches $16.1 billion, and it is estimated that in 2017 reaches $17.2 billion, wherein the market share of the chinese polishing material in 2016 is about 20% of the world, and the market size is about 23 billion renmins. The market capacity of the polishing material mainly depends on the output of the downstream wafers, keeps steadily increasing in recent years, can be expected to keep the annual average growth rate of 4% in the future, reaches over 19 hundred million dollars in the global market scale of 2020, and is expected to break through 12 hundred million dollars in the market scale of 2020, thus being a main motive power for driving the market growth of polishing consumables.
Ceria forms a Ce-O-Si structure with silicon oxide, and has a high reactivity with silicon dioxide to provide a high polishing Removal Rate (RR), and is widely used for polishing of an interlayer insulating layer. For example, in a 3d nand architecture memory chip, the oxide layer is typically thicker than 3 microns. To maintain the throughput requirements, polishing must be performed at very high speeds. Referring to the literature, it is known that: the 111 surface of cerium oxide having high polishing performance has the highest performance. And yttrium-doped cerium oxide is favorable for the growth of the 111 surface.
The properties of the cerium oxide particles determine the polishing performance. For example, in STI polishing applications, cerium oxide crystal structure, particle size, morphology, degree of agglomeration, particle size distribution all have important effects on defect generation during polishing, polishing rate, and selectivity. The conventional high-temperature roasting method for synthesizing cerium oxide has the problems of particle sintering and agglomeration, and cerium oxide powder needs to be subjected to ball milling and dispersing treatment to meet the application requirements of CMP (chemical mechanical polishing), so that the requirements on synthesizing and dispersing equipment and technology are high.
Chinese publication No. CN101641289a discloses a method for preparing cerium carbonate powder by mixing a cerium precursor solution with a urea solution and performing a precipitation reaction. By using organic solvent as cerium precursor solution and urea solution, the reaction temperature of the system is increased to 120 ℃ to precipitate, hexagonal cerium carbonate is prepared, and cerium oxide is prepared by roasting.
Chinese publication No. CN105800664a discloses a reaction between cerium nitrate and ammonium carbonate, after the pH value of the mixed precipitate sample is adjusted to 8.0, the mixed system is subjected to hydrothermal crystallization reaction at 100 ℃ for 12 hours, the obtained precipitate is washed 3 times by pure water, and the obtained precipitate is filtered to obtain a filter cake, and the filter cake is dried to obtain hexagonal phase basic cerium carbonate powder.
Chinese publication No. CN105800661a discloses a method for obtaining cerium hydroxide by mixing a precipitant, a cerium source and an oxidizing agent, and precipitating, wherein, the precipitant is added into a cerium source solution first, stirring is maintained, and when the pH of a precipitation mixture reaches 7.0-10.0, the addition of the precipitant is stopped; and adding an oxidant solution into the precipitation mixed solution to precipitate to obtain cerium hydroxide. Cerium hydroxide is subjected to hydrothermal synthesis reaction to prepare cerium oxide particles.
The hydrothermal method is one of important methods for synthesizing the nano material, and at present, a technology for directly synthesizing the cerium oxide nano material by adopting the hydrothermal method is lacked.
Disclosure of Invention
The invention aims to provide a preparation method of a cerium-yttrium grinding material for CMP, the prepared cerium-yttrium grinding material is specially used for chemical mechanical polishing in the preparation process of semiconductors, the cerium-yttrium grinding material has high purity, the content of metal sodium ions is less than 0.5ppm, the dispersibility is good, the particles are uniform, and the grinding efficiency is high.
In order to achieve the above purpose, the technical solution adopted by the invention is as follows:
the preparation method of the cerium yttrium grinding material for CMP comprises the following steps:
respectively dissolving soluble salts of cerium and yttrium, mixing to obtain yttrium-cerium mixed solution, and preparing cerium-yttrium hydroxide by adopting a homogeneous coprecipitation method;
oxidizing low-valence cerium in cerium yttrium hydroxide into high-valence cerium, filtering reactants, putting a filter cake into a high-pressure reaction kettle, and performing hydrothermal reaction to obtain oxides of cerium and yttrium serving as cerium yttrium grinding materials; the content of yttrium oxide is 0.5-15 w% of the total amount of rare earth oxide, and the content of cerium oxide is 88-99.5 w% of the total amount of rare earth oxide.
Preferably, the soluble salt is selected from nitrate, chloride, sulfate, acetate, and citrate.
Preferably, the precipitant is urea or ammonia water.
Preferably, cerium nitrate and yttrium nitrate are respectively dissolved, and the two solutions are mixed according to the mole ratio of Y 2 O 3 ：CeO 2 Mixing the above materials according to a set ratio of 0.5-1:5.9-7 to obtain yttrium cerium mixed nitric acid solution, and coprecipitating the yttrium cerium hydroxide solution by using ammonia water as a precipitator.
Preferably, cerium nitrate and yttrium nitrate are respectively dissolved, and the two solutions are mixed according to the mole ratio of Y 2 O 3 ：CeO 2 Mixing the materials in a set proportion of (0.5-1:5.9-7) to obtain yttrium cerium mixed nitric acid solution; firstly, adjusting pH=3-4 by using ammonia water to mix yttrium cerium mixed nitric acid solution, and according to REO: CO (H) 2 N) 2 Urea is added in the proportion of 1:2-2.5, and cerium yttrium hydroxide is prepared by homogeneous precipitation at the constant temperature of 80-85 ℃.
Preferably, the homogeneous coprecipitation uses a re-agglomeration-preventing surfactant, and the surfactant is an anionic surfactant, a nonionic surfactant or a combination of the anionic surfactant and the nonionic surfactant; the anionic surfactant is selected from: sodium polyacrylate, ammonium polyacrylate, sodium dodecyl sulfate, sodium hexadecyl sulfate, sodium octadecyl sulfate, sodium dioctyl succinate sulfonate, sodium dodecyl benzene sulfonate; the nonionic surfactant is selected from: polyethylene glycol, nonylphenol polyoxyethylene ether, and octylphenol polyoxyethylene ether.
Preferably, the lower cerium in the cerium yttrium hydroxide is oxidized to higher cerium by air or by an oxidizing agent.
Preferably, the cerium oxide is a mixed oxide of trivalent cerium and tetravalent cerium, wherein the content of tetravalent cerium is not less than 90% of the total cerium, and the addition of the auxiliary agent to the oxide of cerium and yttrium yields the finished polishing powder or slurry.
The technical effects of the invention include:
the invention does not need to adopt the traditional precipitation roasting grinding procedure, prepares cerium yttrium polishing slurry for integrated circuit chemical mechanical polishing by homogeneous coprecipitation and hydrothermal method, and is specially used for chemical mechanical polishing in the semiconductor preparation process. The prepared cerium yttrium grinding material has high purity of cerium yttrium oxide, less than 0.5ppm of metal sodium ion, good dispersibility, uniform particles and high grinding efficiency.
The cerium yttrium grinding material prepared by the invention has no secondary pollution in the reaction process.
Drawings
FIG. 1 is an XRD (X-ray diffraction) diffraction pattern of a cerium yttrium abrasive material prepared in the present invention;
FIG. 2 is a graph showing the particle size distribution of cerium yttrium abrasive materials prepared in accordance with the present invention.
Detailed Description
The following description fully illustrates the specific embodiments of the invention to enable those skilled in the art to practice and reproduce it.
The preparation method of the cerium yttrium grinding material for CMP comprises the following specific steps:
step 1: respectively dissolving soluble salts of cerium and yttrium, mixing to obtain yttrium-cerium mixed solution, and preparing cerium-yttrium hydroxide by adopting a homogeneous coprecipitation method;
in the preferred embodiment, nitrate of cerium and yttrium is selected. The soluble salt is selected from nitrate, chloride, sulfate, acetate and citrate. The precipitant is selected from: urea or ammonia, or a combination of both.
The homogeneous coprecipitation method adopts the following two modes, and the following concrete steps are adopted:
(1) Cerium nitrate (Y) 2 O 3 TREO (total rare earth oxides) 99.999% or more), yttrium nitrate (CeO) 2 Dissolving TREO (total rare earth oxide) not less than 99.99%, respectively, and mixing the two solutions at a molar ratio of Y 2 O 3 ：CeO 2 Mixing the above materials according to a set ratio of 0.5-1:5.9-7 to obtain yttrium cerium mixed nitric acid solution, and using ammonia (NH 3 H 2 O) is a precipitator for coprecipitation to prepare the cerium yttrium hydroxide.
(2) Cerium nitrate (Y) 2 O 3 TREO (total rare earth oxides) 99.999% or more), yttrium nitrate (CeO) 2 Dissolving TREO not less than 99.99%, respectively, and mixing the two solutions at a molar ratio of Y 2 O 3 ：CeO 2 Mixing the materials in a set proportion of (0.5-1:5.9-7) to obtain yttrium cerium mixed nitric acid solution; firstly, adjusting pH=3-4 by using 1:3 ammonia water to prepare a yttrium cerium mixed nitric acid solution according to REO (rare earth element oxide): CO (H) 2 N) 2 Adding urea into the mixture in the ratio (w/w) of (urea) =1:2-2.5, carrying out homogeneous precipitation at the constant temperature of 80-85 ℃, and adding a reagglomeration-preventing surfactant if necessary to prepare the cerium yttrium hydroxide.
The surfactant is selected from anionic surfactant, nonionic surfactant or their combination.
The anionic surfactant is selected from: sodium polyacrylate, ammonium polyacrylate, sodium dodecyl sulfate, sodium hexadecyl sulfate, sodium octadecyl sulfate, sodium dioctyl succinate sulfonate, and sodium dodecyl benzene sulfonate.
The nonionic surfactant is selected from: polyethylene glycol, nonylphenol polyoxyethylene ether, and octylphenol polyoxyethylene ether.
In the homogeneous coprecipitation method, the chemical reaction formula involved is as follows:
CO(H 2 N) 2 +3H 2 O＝2NH 3 H 2 O+CO 2
NH 3 H 2 O＝NH 4 + +OH -
Ce 3+ +3OH - ＝Ce(OH) 3
Y 3+ +3OH - ＝Y(OH )3
step 2: oxidizing low valence cerium in cerium yttrium hydroxide into high valence cerium, filtering reactants, putting a filter cake into a high pressure reaction kettle, and performing pressurized hydrothermal reaction to obtain oxides of cerium and yttrium serving as cerium yttrium grinding materials.
Cerium and yttrium oxide as cerium-yttrium grinding material, yttrium oxide accounting for 0.5-15% of the total amount of the rare earth oxide (REO/TREO), and cerium oxide accounting for 88-99.5% of the total amount of the rare earth oxide
(REO/TREO). The cerium oxide is a mixture of high cerium and low cerium, and is a mixed oxide of trivalent cerium and tetravalent cerium, wherein the content of tetravalent cerium accounts for not less than 90% of the total cerium. And adding an auxiliary agent into the oxide of cerium and yttrium to obtain finished polishing powder or polishing slurry.
In the present invention, air or an oxidizing agent (H 2 O 2 ) The lower cerium in the cerium yttrium hydroxide is oxidized to higher cerium. The cerium hydroxide in the cerium yttrium hydroxide is high cerium hydroxide (Ce (OH) 4 ) Or ceric hydroxide and low cerium hydroxide (Ce (OH) 3 ) Is a mixture of (a) and (b).
Oxidizing the low valence cerium with hydrogen peroxide to oxidize the low valence cerium to high valence cerium: cooling to 20 ℃, and the molar ratio REO: h 2 O 2 =1: hydrogen peroxide (concentration 30 wt%) was added in a ratio of 1.5; heating the reaction product to 95 ℃ and boiling for 30 minutes; filtering, washing with water for 2 times, putting the filter cake into a high-pressure reaction kettle, pressurizing with 150-170Kg pressure, performing hydrothermal reaction for 120 minutes, and filtering the product with a 0.5 μm filter element to obtain polishing slurry.
The chemical reaction formula involved is as follows:
Ce(OH) 4 +H 2 O 2 ＝Ce(OH) 3 (OOH)+H 2 O
2Ce(OH) 3 (OOH)＝2Ce(OH) 4 +O 2
Ce(OH) 4 ＝CeO 2 ·+2H 2 O
example 1
Solution Y (NO) with reo=100 g/L was prepared separately 3 ) 3 、Ce(NO 3 ) 3 The solution is prepared into a liquid preparation,
(Y 2 O 3 /TREO＝99.999％，CeO 2 treo=99.98%). 4000ml Ce (NO) 3 ) 3 The solution was adjusted to ph=3 by adding aqueous ammonia (6%, wt%). In a molar ratio of Y 2 O 3 ：CeO 2 =1: a ratio of 5.9 will be 42mlY (NO 3 ) 3 Added to Ce (NO) 3 ) 3 Among the solutions, this mixed solution is denoted as solution α (yttrium cerium mixed nitric acid solution).
In a constant temperature water bath at 80℃450g of urea was added to a beaker containing 5000ml of deionized water, 8g of polyethylene glycol (PEG-400), 5g of ammonium polyacrylate, which was precipitant beta.
Dropping the precipitant beta into the solution alpha at the speed of 50ml/min, and filtering the precipitate after the reaction is completed.
The precipitate was rinsed with 2000ml deionized water, with 200ml ammonia (5 mol/L) and 170gH 2 O 2 The solution (30% by weight) oxidizes the lower cerium in the cerium yttrium hydroxide to higher cerium, and is stirred for 20 minutes, heated to 95 ℃ and boiled for 30 minutes. Filtered and washed 2 times with 2000ml deionized water. Suction filtration, put the filter cake into a high-pressure reaction kettle, and carry out hydrothermal reaction under 170Kg pressure for 120 minutes. Naturally cooling, and filtering with 0.5 μm filter core to obtain the final product.
Example 2
The raw materials used were the same as in example 1.
12g of polyethylene glycol (PEG-400) was added and heated to 50 ℃. 2000ml of 10% aqueous ammonia solution was prepared, and aqueous ammonia was added dropwise to the raw material liquid while stirring at a constant temperature. Cooled to 20 ℃ and 170gH is added 2 O 2 The solution (30% by weight) oxidizes the lower cerium in the cerium yttrium hydroxide to higher cerium, and is stirred for 20 minutes, heated to 95 ℃ and boiled for 30 minutes. Filtered and washed 2 times with 2000ml deionized water. Filtering, putting the filter cake into a high-pressure reaction kettle, and carrying out pressurized hydrothermal reaction for 6 hours under 150Kg pressure to obtain the oxides of cerium and yttrium.
Example 3
1000ml Ce (NO) 3 ) 3 Solution(REO＝100g/L，CeO 2 After precipitation was completed, the lower cerium in the cerium-yttrium hydroxide was oxidized to higher cerium by air (500 ml/min) with stirring by air pump until the color was no longer darkened. 2000ml deionized water was added and washed once, and filtered. Adding the filter cake into a high-pressure reaction kettle, adding 1000ml of deionized water, and carrying out hydrothermal reaction at 170 ℃ for 6 hours to obtain the cerium and yttrium oxide products.
As shown in fig. 1, an XRD (X-ray diffraction) diffraction pattern of the cerium yttrium abrasive material prepared in the present invention.
Cerium yttrium abrasive material, its X-ray diffraction characteristic peaks 2 theta are 28.78, 47.86, 70.05, 77.3. The cerium yttrium grinding material is a better crystalline substance and has higher polishing performance. The diffraction peak of cerium yttrium oxide is shifted to a large angle by 0.25 degrees compared with the characteristic peak of pure cerium, and the lattice constant becomes smaller, which indicates that yttrium ions and cerium ions form a substituted solid solution.
As shown in FIG. 2, the particle size distribution diagram of the cerium yttrium abrasive material prepared in the present invention is shown.
The cerium-yttrium abrasive material has uniform and dispersed cerium oxide and yttrium oxide particles and high purity.
Reference example 1
2000ml Ce (NO) 3 ) 3 Solution (100 g/L CeO) 2 TREO=99.98%, 500ml of aqueous ammonia (5 mol/L) were added, 300g H were added with stirring 2 O 2 The solution (30% wt%) was reacted for 30 minutes and heated to boil. After natural cooling, the mixture was filtered and the filter cake was washed 2 times with 2000ml deionized water. Filtering, adding the filter cake into a high-pressure reaction kettle, adding 1000ml of deionized water, and carrying out hydrothermal reaction at 150 ℃ for 6 hours. After cooling, ph=8 was adjusted with 1:10 ammonium hydroxide, which is reference 1.
Reference example 2
2000ml Ce (NO) 3 ) 3 The solution (100 g/L, ceO 2/treo=99.98%) was boiled with maintaining the boiling, 200g of ammonium bicarbonate was added. After the precipitation was completed, the solution was filtered and washed with water 2 times with 2000ml of water each time. Filtering, drying at 120deg.C, and calcining at 580 deg.C in muffle furnaceAnd 6 hours. The fired product was taken out and slurried with water (10 wt%). The particles were ground to a particle size d50=0.1 μm using a zeta@rs 4L sand mill, which is reference example 2.
Polishing test conditions
All the above samples were taken to prepare polishing slurries with a solids content of 5% and ph=8. The polishing equipment used in the experiment isThe wafer slices used for MESA CMP 200MM were obtained from commercially available 200MM coated wafer slices. TEOS thickness was measured by RT-7O/RG-7B (NAPSON, inc.) and the polishing pad was a ceramic IC1010. The experimental parameters were set as follows: the polishing slurry flow rate was 120mL/min, the downward pressure was 4psi, the turntable speed/polishing head speed = 50/70rpm, and the polishing time was 45s.
TABLE 1 polishing Rate of abrasive materials
The terminology used herein is for the purpose of description and illustration only and is not intended to be limiting. As the present invention may be embodied in several forms without departing from the spirit or essential attributes thereof, it should be understood that the above-described embodiments are not limited by any of the details of the foregoing description, but rather should be construed broadly within its spirit and scope as defined in the appended claims, and therefore all changes and modifications that fall within the metes and bounds of the claims, or equivalences of such metes and bounds are therefore intended to be embraced by the appended claims.
Claims (8)
1. A method for preparing cerium yttrium abrasive material for CMP, comprising:
respectively dissolving soluble salts of cerium and yttrium, mixing to obtain yttrium-cerium mixed solution, and preparing cerium-yttrium hydroxide by adopting a homogeneous coprecipitation method;
oxidizing low-valence cerium in cerium yttrium hydroxide into high-valence cerium, filtering reactants, putting a filter cake into a high-pressure reaction kettle, and performing hydrothermal reaction to obtain oxides of cerium and yttrium serving as cerium yttrium grinding materials; the content of yttrium oxide is 0.5-15 w% of the total amount of rare earth oxide, and the content of cerium oxide is 88-99.5 w% of the total amount of rare earth oxide.
2. The method for preparing cerium-yttrium abrasive material for CMP according to claim 1, wherein the soluble salt is selected from nitrate, chloride, sulfate, acetate, and citrate.
3. The method for preparing a cerium-yttrium abrasive material for CMP according to claim 1, wherein the precipitant is urea or ammonia water.
4. The method for producing a cerium-yttrium abrasive material for CMP according to claim 1, wherein cerium nitrate and yttrium nitrate are dissolved separately, and the two solutions are mixed in a molar ratio of Y 2 O 3 ：CeO 2 Mixing the above materials according to a set ratio of 0.5-1:5.9-7 to obtain yttrium cerium mixed nitric acid solution, and coprecipitating the yttrium cerium hydroxide solution by using ammonia water as a precipitator.
5. The method for producing a cerium-yttrium abrasive material for CMP according to claim 1, wherein cerium nitrate and yttrium nitrate are dissolved separately, and the two solutions are mixed in a molar ratio of Y 2 O 3 ：CeO 2 Mixing the materials in a set proportion of (0.5-1:5.9-7) to obtain yttrium cerium mixed nitric acid solution; firstly, adjusting pH=3-4 by using ammonia water to mix yttrium cerium mixed nitric acid solution, and according to REO: CO (H) 2 N) 2 Urea is added in the proportion of 1:2-2.5, and cerium yttrium hydroxide is prepared by homogeneous precipitation at the constant temperature of 80-85 ℃.
6. The method for preparing cerium-yttrium abrasive material for CMP according to claim 1, wherein a re-agglomeration preventing surfactant is used in homogeneous coprecipitation, and the surfactant is selected from anionic surfactant, nonionic surfactant or a combination of both surfactants; the anionic surfactant is selected from: sodium polyacrylate, ammonium polyacrylate, sodium dodecyl sulfate, sodium hexadecyl sulfate, sodium octadecyl sulfate, sodium dioctyl succinate sulfonate, sodium dodecyl benzene sulfonate; the nonionic surfactant is selected from: polyethylene glycol, nonylphenol polyoxyethylene ether, and octylphenol polyoxyethylene ether.
7. The method for producing a cerium-yttrium abrasive material for CMP according to claim 1, wherein the lower cerium in cerium-yttrium hydroxide is oxidized to higher cerium by air or by an oxidizing agent.
8. The method for preparing a cerium-yttrium abrasive material for CMP according to claim 1, wherein the cerium oxide is a mixed oxide of trivalent cerium and tetravalent cerium, wherein the content of tetravalent cerium is not less than 90% of the total cerium, and an auxiliary agent is added to the oxide of cerium and yttrium to obtain a finished polishing powder or slurry.
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