CN118725745A - Dispersion and use thereof - Google Patents
Dispersion and use thereof Download PDFInfo
- Publication number
- CN118725745A CN118725745A CN202310366812.7A CN202310366812A CN118725745A CN 118725745 A CN118725745 A CN 118725745A CN 202310366812 A CN202310366812 A CN 202310366812A CN 118725745 A CN118725745 A CN 118725745A
- Authority
- CN
- China
- Prior art keywords
- cerium oxide
- dispersion
- cerium
- oxide particles
- planarization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000006185 dispersion Substances 0.000 title claims abstract description 156
- 229910000420 cerium oxide Inorganic materials 0.000 claims abstract description 233
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims abstract description 233
- 239000002245 particle Substances 0.000 claims abstract description 174
- 239000007788 liquid Substances 0.000 claims abstract description 63
- 239000000203 mixture Substances 0.000 claims abstract description 61
- 238000004435 EPR spectroscopy Methods 0.000 claims abstract description 42
- 239000002904 solvent Substances 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims description 56
- 239000007787 solid Substances 0.000 claims description 48
- 239000002244 precipitate Substances 0.000 claims description 41
- 238000002834 transmittance Methods 0.000 claims description 35
- 239000011259 mixed solution Substances 0.000 claims description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 31
- 238000002360 preparation method Methods 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000013078 crystal Substances 0.000 claims description 23
- 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 22
- 238000002441 X-ray diffraction Methods 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000011521 glass Substances 0.000 claims description 15
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 12
- 235000012239 silicon dioxide Nutrition 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 12
- 239000006228 supernatant Substances 0.000 claims description 11
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 8
- 150000000703 Cerium Chemical class 0.000 claims description 8
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 7
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 6
- 150000007530 organic bases Chemical class 0.000 claims description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- WTKZEGDFNFYCGP-UHFFFAOYSA-N Pyrazole Chemical compound C=1C=NNC=1 WTKZEGDFNFYCGP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- HKVFISRIUUGTIB-UHFFFAOYSA-O azanium;cerium;nitrate Chemical compound [NH4+].[Ce].[O-][N+]([O-])=O HKVFISRIUUGTIB-UHFFFAOYSA-O 0.000 claims description 3
- 125000004432 carbon atom Chemical group C* 0.000 claims description 3
- PYPNFSVOZBISQN-LNTINUHCSA-K cerium acetylacetonate Chemical compound [Ce+3].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O PYPNFSVOZBISQN-LNTINUHCSA-K 0.000 claims description 3
- 229960001759 cerium oxalate Drugs 0.000 claims description 3
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 3
- ZMZNLKYXLARXFY-UHFFFAOYSA-H cerium(3+);oxalate Chemical compound [Ce+3].[Ce+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZMZNLKYXLARXFY-UHFFFAOYSA-H 0.000 claims description 3
- 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 3
- 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 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 3
- 239000003002 pH adjusting agent Substances 0.000 claims description 3
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 3
- 229920005591 polysilicon Polymers 0.000 claims description 3
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 3
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 238000005498 polishing Methods 0.000 description 44
- 230000000694 effects Effects 0.000 description 29
- 230000008569 process Effects 0.000 description 26
- 238000000227 grinding Methods 0.000 description 23
- 230000007547 defect Effects 0.000 description 20
- 235000019441 ethanol Nutrition 0.000 description 13
- 239000005304 optical glass Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- 229910052684 Cerium Inorganic materials 0.000 description 8
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 8
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 8
- 239000000084 colloidal system Substances 0.000 description 8
- 230000036571 hydration Effects 0.000 description 8
- 238000006703 hydration reaction Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 229910021642 ultra pure water Inorganic materials 0.000 description 8
- 239000012498 ultrapure water Substances 0.000 description 8
- 230000009286 beneficial effect Effects 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000002296 dynamic light scattering Methods 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 description 5
- 230000002349 favourable effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- KWIUHFFTVRNATP-UHFFFAOYSA-N glycine betaine Chemical compound C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 description 4
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- -1 triethylamine alcohol amine Chemical class 0.000 description 4
- 239000003082 abrasive agent Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 229910052814 silicon oxide Inorganic materials 0.000 description 3
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 125000004429 atom Chemical group 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229960003237 betaine Drugs 0.000 description 2
- 239000011246 composite particle Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000000087 laser glass Substances 0.000 description 2
- 239000000693 micelle Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000005118 spray pyrolysis Methods 0.000 description 2
- 229940117986 sulfobetaine Drugs 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910001428 transition metal ion Inorganic materials 0.000 description 2
- 239000004471 Glycine Substances 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- ONIBWKKTOPOVIA-BYPYZUCNSA-N L-Proline Chemical compound OC(=O)[C@@H]1CCCN1 ONIBWKKTOPOVIA-BYPYZUCNSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 229920002873 Polyethylenimine Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- ONIBWKKTOPOVIA-UHFFFAOYSA-N Proline Natural products OC(=O)C1CCCN1 ONIBWKKTOPOVIA-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- HNDVDQJCIGZPNO-UHFFFAOYSA-N histidine Natural products OC(=O)C(N)CC1=CN=CN1 HNDVDQJCIGZPNO-UHFFFAOYSA-N 0.000 description 1
- 230000007954 hypoxia Effects 0.000 description 1
- 229940094506 lauryl betaine Drugs 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- DVEKCXOJTLDBFE-UHFFFAOYSA-N n-dodecyl-n,n-dimethylglycinate Chemical compound CCCCCCCCCCCC[N+](C)(C)CC([O-])=O DVEKCXOJTLDBFE-UHFFFAOYSA-N 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
- B24B37/07—Lapping machines or devices; Accessories designed for working plane surfaces characterised by the movement of the work or lapping tool
- B24B37/10—Lapping machines or devices; Accessories designed for working plane surfaces characterised by the movement of the work or lapping tool for single side lapping
-
- 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
- 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
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Power Engineering (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Computer Hardware Design (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
An embodiment of the present application provides a dispersion liquid including a first solvent and cerium oxide particles dispersed in the first solvent, wherein the cerium oxide particles have an electron spin resonance signal peak, and a peak position of the electron spin resonance signal peak is less than or equal to 2.05. The dispersion of the embodiments of the present application can be used to prepare planarization compositions that increase the planarization rate without increasing the particle size of the cerium oxide particles.
Description
Technical Field
The embodiment of the application relates to the technical field of planarization, in particular to a dispersion liquid and application thereof.
Background
At present, cerium oxide is widely reported as an abrasive for planarization process of semiconductor manufacturing. It is of great interest mainly due to the high abrasive removal activity of cerium oxide on silica and it achieves high abrasive removal at lower solids content. Therefore, the planarization composition using cerium oxide as an abrasive has a wider application prospect and market advantage in terms of performance and cost than the traditional silicon oxide or aluminum oxide materials.
In polishing liquids in which cerium oxide is used as an abrasive, the particle characteristics of cerium oxide are important for the effect of polishing. For example, in dielectric layer planarization applications, cerium oxide particle size, morphology, etc., have important effects on both defect generation and polishing removal rate selection during planarization. In planarization applications, surface scratch defects are mainly caused by large particles in the slurry, however, if small particle size abrasives are used, this will result in loss of the removal rate. In the prior art, surface scratch and polishing removal rate are very important measures of polishing effect. Therefore, how to increase the polishing removal rate without increasing the particle size is a difficult problem in the synthesis of the cerium oxide abrasive.
Disclosure of Invention
In view of this, the embodiments of the present application provide a dispersion and an application thereof, the dispersion is a colloidal cerium oxide material, and the dispersion can be used as an abrasive in a planarization process, so as to increase the polishing removal rate without increasing the particle size of cerium oxide particles, thereby solving the problem that the polishing removal rate is low for reducing surface scratches in the prior art.
Specifically, a first aspect of the embodiment of the present application provides a dispersion liquid including a first solvent and cerium oxide particles dispersed in the first solvent, wherein the cerium oxide particles have an electron spin resonance signal peak, and a peak position of the electron spin resonance signal peak is less than or equal to 2.05. The embodiment of the present application can improve the polishing removal rate without increasing the particle diameter of cerium oxide particles by controlling the signal peak position of electron spin resonance of cerium oxide particles in a dispersion to a value of 2.05 or less. Among them, electron spin resonance (electron spin resonance, ESR) is a method for examining a substance containing unpaired electrons, and the detection target includes radicals, transition metal ions, multi-state molecules, crystal defects, and the like. Electron spin resonance can identify the information of valence state of single electron substances, nature of adjacent atoms, symmetry of surface parts, total number of unpaired spin electrons in the unit catalyst and the like in the catalyst. The electron spin resonance signal peak is the g factor, and the g factor can represent the information of unpaired electron environment and is an important index for representing crystal defects. The signal peak of electron spin resonance can be obtained by using electron spin resonance spectrometer.
In an embodiment of the present application, the X-ray diffraction angle 2θ corresponding to the (111) crystal plane of the cerium oxide particles is less than or equal to 28.6 °. The embodiment of the present application can improve the polishing removal rate without increasing the particle diameter of the cerium oxide particles by controlling the X-ray diffraction angle 2 theta corresponding to the (111) crystal plane of the cerium oxide particles in the dispersion to a value of 28.6 deg. or less, mainly because the cerium oxide particles can be made to have more lattice defects including oxygen vacancy defects, the presence of which in the cerium oxide will cause the global potential to be unbalanced, part of the tetravalent cerium will become trivalent cerium, and the presence of trivalent cerium will improve the polishing removal rate. The angle value of the X-ray diffraction angle 2θ corresponding to the (111) crystal plane of the cerium oxide particles can be obtained by an X-ray diffractometer test.
In an embodiment of the application, the pH of the dispersion is in the range of 2.0 to 4.0. The pH value of the dispersion liquid is controlled to be 2.0-4.0, which is favorable for obtaining cerium oxide particles with the signal peak position of electron spin resonance smaller than or equal to 2.05, for obtaining cerium oxide particles with the X-ray diffraction angle 2 theta corresponding to a (111) crystal face smaller than or equal to 28.6 degrees, and for reducing the hydration particle size of the cerium oxide particles, so that the dispersibility of the cerium oxide particles in the dispersion liquid is improved, the flattening operation is facilitated, and the preservation is facilitated.
In an embodiment of the application, the pH of the dispersion is in the range of 2.0 to 3.0. The pH value of the dispersion liquid is controlled to be 2.0-3.0, so that cerium oxide particles with the signal peak position of electron spin resonance smaller than or equal to 2.05 can be better obtained, cerium oxide particles with the X-ray diffraction angle 2 theta corresponding to a (111) crystal face smaller than or equal to 28.6 DEG can be better obtained, the hydration particle size of the cerium oxide particles can be reduced, the dispersibility of the cerium oxide particles in the dispersion liquid can be improved, the flattening operation can be facilitated, and the preservation can be facilitated.
In the embodiment of the application, the hydration particle size of the cerium oxide particles is nano-scale, namely the cerium oxide nano-particles. The hydrated particle size of the cerium oxide particles is the particle size of the composite particles in the state of a solution and is a hydrodynamic diameter, and the hydrated particle size of the cerium oxide particles comprises a core of the cerium oxide particles and an expanded micelle. The cerium oxide particles have nano-scale hydrated particle size, namely small size, which is beneficial to reducing the scratch defect of the surface of the flattened object in the flattening process, thereby improving the grinding effect. The hydrated particle diameter of the cerium oxide particles can be measured by a dynamic light scattering (DYNAMIC LIGHT SCATTERING, DLS) method, specifically, after the diffusion coefficient D of the cerium oxide particles is obtained, the hydrated diameter of the cerium oxide particles can be obtained according to Stokes-Einstein equation:
Stokes-Einstein equation:
Wherein D is a diffusion coefficient, and k B is a Boltzmann constant; t is absolute temperature; η 0 is the viscosity of the system; d is the hydrodynamic diameter, i.e., the hydration diameter.
In an embodiment of the present application, the cerium oxide particles have a hydrated particle size of 50nm or less. The cerium oxide particles have smaller-sized hydrated particle sizes smaller than or equal to 50nm, so that the generation of scratch defects on the surface of the flattened object in the flattening process can be reduced better, and the grinding effect is improved.
In an embodiment of the application, the dispersion has an average light transmittance of less than 5% for light having a wavelength of 190nm to 370nm when the solids content is adjusted to 0.3% by weight. The dispersion has an average light transmittance of less than 5% at a solid content of 0.3% by weight with respect to light having a wavelength of 190nm to 370nm, and can be used as an abrasive for planarization to improve polishing effect.
In an embodiment of the application, the dispersion has an average transmittance of less than or equal to 2.5% for light having a wavelength of 190nm to 370nm when the solids content is adjusted to 0.3% by weight. The smaller average light transmittance indicates that the solid particles in the dispersion are small and dispersed very uniformly, thereby further facilitating the improvement of the grinding effect when used as an abrasive in the planarization process.
In an embodiment of the application, the dispersion has an average transmittance of less than 0.01% for light having a wavelength of 190nm to 320nm when the solids content is adjusted to 0.3% by weight. The dispersion has an average light transmittance of less than 0.01% at a solid content of 0.3% by weight with respect to light having a wavelength of 190nm to 320nm, and can be used as an abrasive for planarization to improve polishing effect.
In an embodiment of the application, the dispersion has an average transmittance of less than or equal to 0.005% for light having a wavelength of 190nm to 320nm when the solids content is adjusted to 0.3% by weight. The smaller average light transmittance indicates that the solid particles in the dispersion are small and dispersed very uniformly, thereby further facilitating the improvement of the grinding effect when used as an abrasive in the planarization process.
In an embodiment of the application, the solids content of the dispersion is 1% to 5% by weight. Suitable solids content control not only facilitates preservation of the dispersion but also subsequent addition to the slurry system.
The dispersion liquid provided by the embodiment of the application can be used as an abrasive for preparing the grinding liquid, the abrasive is a colloidal nano cerium oxide abrasive with small size, rich defects and high activity, and the grinding liquid prepared by adopting the abrasive is used for flattening a dielectric layer, so that higher grinding removal rate and lower surface scratch can be obtained, and the grinding effect is improved.
In a second aspect, the present embodiment provides a method for preparing a dispersion, including:
Adding soluble cerium salt into organic alcohol or a mixture of organic alcohol and water to obtain a mixed solution, adding organic alkali into the mixed solution to form a precipitate in the mixed solution to obtain a precipitate mixture, removing supernatant in the precipitate mixture, and adding a first solvent to obtain a dispersion; in the preparation process, a pH regulator is adopted to regulate the pH of the system, so that the pH of the dispersion liquid is 2.0-4.0; the dispersion liquid comprises a first solvent and cerium oxide particles dispersed in the first solvent, wherein the signal peak position of electron spin resonance of the cerium oxide particles is less than or equal to 2.05.
According to the preparation method of the dispersion liquid, the preparation of the colloidal cerium oxide with the signal peak position of electron spin resonance of cerium oxide particles smaller than or equal to 2.05 can be realized by selecting specific reaction raw materials and reaction solvents and carrying out specific regulation and control on the pH value of a system, and the prepared colloidal cerium oxide can be used as an abrasive in the planarization process, so that the polishing removal rate is improved under the condition of not increasing the particle size of cerium oxide particles; the preparation method of the dispersion liquid provided by the embodiment of the application has the advantages of simple process and easiness in realizing industrial production.
In an embodiment of the present application, the soluble cerium salt includes one or more of cerium nitrate, cerium sulfate, ammonium cerium nitrate, cerium chloride, cerium acetate, cerium oxalate, and cerium acetylacetonate. The soluble cerium salt may provide a source of cerium for the reaction system.
In an embodiment of the present application, the organic alcohol includes monohydric alcohols having 1 to 10 carbon atoms. Specifically, examples include methanol, ethanol, n-propanol, isopropanol, n-butanol, n-pentanol, and isopentanol.
In an embodiment of the present application, the organic base includes one or more of ammonia water, ethanolamine, diethanolamine, triethanolamine, imidazole, pyridine, pyrazole, diethylamine, and triethylamine alcohol amine.
In an embodiment of the application, the pH adjuster comprises nitric acid. Nitric acid is used as a pH regulator, so that the method is beneficial to being suitable for application scenes of dielectric layer planarization.
In a third aspect, embodiments of the present application provide a planarization composition comprising the dispersion of the first aspect of embodiments of the present application and a second solvent.
In an embodiment of the present application, the planarization composition further includes an additive. The additives may be added according to actual needs.
In an embodiment of the present application, the planarization composition has a pH of 4.0 to 7.0.
A fourth aspect of the present application provides a dispersion according to the first aspect of the present application or a use of a planarization composition according to the third aspect of the present application for planarizing a dielectric layer.
In the embodiment of the application, the dielectric layer may be a dielectric material layer commonly used in the field of electronic manufacturing, and may include a silicon dioxide layer, a silicon nitride layer and a polysilicon layer, for example.
Embodiments of the present application also provide a dispersion according to the first aspect of the embodiments of the present application, or a use of a flattening composition according to the third aspect of the embodiments of the present application, in glass flattening. The glass may be, for example, colorless optical glass, colored optical glass, laser glass, quartz optical glass, radiation-resistant glass, ultraviolet-infrared (high-transmittance, absorption) optical glass, fiber optical glass, acousto-optic glass, magneto-optic glass, photochromic glass, photomask glass, and the like.
The embodiment of the application also provides a flattening method, which enables the flattening composition in the third aspect of the embodiment of the application to be in contact with the surface of the object to be flattened and relatively move the object to be flattened.
Drawings
Fig. 1 is a schematic operation of a planarization process.
Detailed Description
Embodiments of the present application will be described below with reference to the accompanying drawings.
The cerium oxide has high grinding removal activity on silicon dioxide, and can realize better grinding effect under lower solid content, so that the grinding liquid taking cerium oxide as an abrasive has wider application prospect and market advantage compared with the traditional silicon oxide or aluminum oxide materials in performance and cost. In a polishing liquid using cerium oxide as an abrasive, particle size, morphological characteristics, and the like of cerium oxide have important effects on the generation of defects in the planarization process and the polishing removal rate. In planarization applications, surface scratch defects are mainly caused by large particles in the slurry, however, the use of small particle size abrasives will result in loss of the removal rate. In the prior process, the surface scratch and the polishing removal rate are very important polishing effect measurement indexes. Therefore, how to increase the polishing removal rate without increasing the particle size is a difficult problem in the synthesis of the cerium oxide abrasive. In order to solve the above problems, the embodiments of the present application provide a dispersion and an application thereof, wherein the dispersion is a colloidal cerium oxide material, and the dispersion can be used as an abrasive in a planarization process, and the polishing removal rate is improved without increasing the particle size of cerium oxide particles, so as to solve the problem that the cerium oxide abrasive in the prior art is low in polishing removal rate because the particle size of cerium oxide particles is continuously reduced to reduce surface scratches.
The embodiment of the application provides a dispersion liquid, namely a cerium oxide dispersion liquid, which comprises a first solvent and cerium oxide particles dispersed in the first solvent, wherein the cerium oxide particles have electron spin resonance signal peaks, and the peak position of the electron spin resonance signal peaks is less than or equal to 2.05. The embodiment of the present application can improve the polishing removal rate without increasing the particle diameter of cerium oxide particles by controlling the peak position of the electron spin resonance signal peak of cerium oxide particles in the cerium oxide dispersion to a value of 2.05 or less. Among them, electron spin resonance (electron spin resonance, ESR) is a method for examining a substance containing unpaired electrons, and the detection target includes radicals, transition metal ions, multi-state molecules, crystal defects, and the like. Electron spin resonance can identify the information of valence state of single electron substances, nature of adjacent atoms, symmetry of surface parts, total number of unpaired spin electrons in the unit catalyst and the like in the catalyst. The electron spin resonance signal peak is the g factor, and the g factor can represent the information of unpaired electron environment and is an important index for representing crystal defects. The signal peak of electron spin resonance can be obtained by using electron spin resonance spectrometer. In the cerium oxide dispersion according to the embodiment of the present application, the peak position of the electron spin resonance signal peak of the cerium oxide particles may be, for example, 2.05, 2.02, 2.00, 1.99, 1.98, 1.97, 1.96, or the like. In some embodiments of the application, the peak position of the electron spin resonance signal peak of the cerium oxide particles in the cerium oxide dispersion is in the range of 1.0 to 2.05.
The cerium oxide dispersion liquid of the embodiment of the application is a colloidal cerium oxide material, in which, dispersoids are cerium oxide particles, a dispersing agent is a first solvent, and the first solvent can be water.
In an embodiment of the present application, the X-ray diffraction angle 2θ corresponding to the (111) crystal plane of the cerium oxide particles is less than or equal to 28.6 °. The embodiment of the present application can improve the polishing removal rate without increasing the particle diameter of the cerium oxide particles by controlling the X-ray diffraction angle 2 theta corresponding to the (111) crystal plane of the cerium oxide particles in the cerium oxide dispersion to a value of 28.6 deg. or less, mainly because the cerium oxide particles can be made to have more lattice defects including oxygen vacancy defects, the presence of which in the cerium oxide will cause the global potential hypoxia imbalance, part of tetravalent cerium will become trivalent cerium, and the presence of trivalent cerium can improve the polishing removal rate. The angle value of the X-ray diffraction angle 2θ corresponding to the (111) crystal plane of the cerium oxide particles can be obtained by an X-ray diffractometer test. In the embodiment of the present application, the X-ray diffraction angle 2θ corresponding to the (111) crystal plane of the cerium oxide particles may be, for example, specifically 28.6 °, 28.5 °, 28.4 °, 28.3 °, 28.2 °, or the like.
In embodiments of the application, the pH of the cerium oxide dispersion may range from 2.0 to 4.0. The pH value of the cerium oxide dispersion liquid is controlled to be 2.0-4.0, which is favorable for obtaining cerium oxide particles with the signal peak position of electron spin resonance smaller than or equal to 2.05, is favorable for obtaining cerium oxide particles with the X-ray diffraction angle 2 theta corresponding to a (111) crystal face smaller than or equal to 28.6 degrees, and is favorable for reducing the hydration particle size of the cerium oxide particles, so that the dispersibility of the cerium oxide particles in the cerium oxide dispersion liquid is improved, the flattening operation is facilitated, and the preservation is favorable.
In some embodiments of the application, the pH of the cerium oxide dispersion is in the range of 2.0 to 3.0. The pH value of the cerium oxide dispersion liquid is controlled to be 2.0-3.0, so that cerium oxide particles with the signal peak position of electron spin resonance smaller than or equal to 2.05 can be better obtained, cerium oxide particles with the X-ray diffraction angle 2 theta corresponding to a (111) crystal face smaller than or equal to 28.6 DEG can be better obtained, the hydration particle size of the cerium oxide particles can be reduced, and the dispersibility of the cerium oxide particles in the cerium oxide dispersion liquid can be improved, and the preservation is facilitated.
In some embodiments of the application, the pH of the cerium oxide dispersion may be, for example, specifically 2.0, 2.2, 2.5, 2.8, 3.0, 3.5, 4.0.
In the embodiment of the application, the hydration particle size of the cerium oxide particles is nano-scale, namely the cerium oxide nano-particles. The hydrated particle size of the cerium oxide particles is the particle size of the composite particles in the state of a solution and is a hydrodynamic diameter, and the hydrated particle size of the cerium oxide particles comprises a core of the cerium oxide particles and an expanded micelle. The cerium oxide particles have a nano-scale hydration particle size, i.e., a small size, which is advantageous for reducing the occurrence of surface scratch defects during the planarization process, thereby improving the polishing effect. The hydrated particle size of the cerium oxide particles can be measured by a dynamic light scattering (DYNAMIC LIGHT SCATTERING, DLS) method, specifically, after the diffusion coefficient D of the cerium oxide particles is obtained, the hydrated particle size of the cerium oxide particles can be obtained according to Stokes-Einstein equation:
Stokes-Einstein equation:
wherein D is a diffusion coefficient, and k B is a Boltzmann constant; t is absolute temperature; η 0 is the viscosity of the system; d is the hydrodynamic diameter, i.e. the hydrated particle size.
In some embodiments of the application, the cerium oxide particles have a hydrated particle size of less than or equal to 50nm. The cerium oxide particles have smaller-sized hydrated particle sizes smaller than or equal to 50nm, so that the generation of scratch defects on the surface of a flattened object (namely the polished object) in the flattening process can be reduced better, and the polishing effect is improved. In some embodiments of the present application, the hydrated particle size of the cerium oxide particles may be, specifically, for example, 50nm, 47nm, 45nm, 40nm, 36nm, 35nm, 30nm, 27nm, 25nm, 20nm, 16nm, 15nm, 10nm, etc.
In an embodiment of the present application, the cerium oxide dispersion has an average transmittance of less than 5% for light having a wavelength of 190nm to 370nm when the solid content is adjusted to 0.3% by weight. In some embodiments, the cerium oxide dispersion has an average light transmittance of 4.5%, 4.0%, 3.5%, 3.0%, 2.5% for light having a wavelength of 190nm to 370nm when the solids content is adjusted to 0.3% by weight. Wherein the solids content refers to the percentage of the weight of the cerium oxide particles in the dry state relative to the total weight of the entire cerium oxide dispersion. The cerium oxide dispersion has an average light transmittance of less than 5% at a solid content of 0.3 wt% with respect to light having a wavelength of 190nm to 370nm, and can be used as an abrasive for planarization to improve polishing effect.
In some embodiments of the application, the cerium oxide dispersion has an average light transmittance of less than or equal to 2.5% for light having a wavelength of 190nm to 370nm when the solids content is adjusted to 0.3% by weight. In some embodiments, the cerium oxide dispersion has an average light transmittance of 2.5%, 2.0%, 1.5%, 1.0%, 0.5%, 0.2%, 0.1% for light having a wavelength of 190nm to 370nm when the solids content is adjusted to 0.3% by weight. The smaller average light transmittance indicates that the cerium oxide solid particles in the cerium oxide dispersion liquid have small particle size and are uniformly dispersed, so that the cerium oxide solid particles are more beneficial to improving the grinding effect when being used as an abrasive in a planarization process.
In an embodiment of the present application, the cerium oxide dispersion has an average transmittance of less than 0.01% for light having a wavelength of 190nm to 320nm when the solid content is adjusted to 0.3% by weight. In some embodiments, the cerium oxide dispersion has an average light transmittance of 0.0095%, 0.009%, 0.0085%, 0.008%, 0.007%, 0.006%, 0.0055% for light having a wavelength of 190nm to 320nm when the solids content is adjusted to 0.3% by weight. The cerium oxide dispersion has an average light transmittance of less than 0.01% at a solid content of 0.3% by weight with respect to light having a wavelength of 190nm to 320nm, and can be used as an abrasive for planarization to improve polishing effect.
In an embodiment of the present application, the cerium oxide dispersion has an average light transmittance of 0.005% or less with respect to light having a wavelength of 190nm to 320nm when the solid content is adjusted to 0.3% by weight. In some embodiments, the cerium oxide dispersion has an average light transmittance of 0.005%, 0.004%, 0.003%, 0.002%, 0.001% for light having a wavelength of 190nm to 320nm when the solids content is adjusted to 0.3% by weight. The smaller average light transmittance indicates that the solid particles in the cerium oxide dispersion have small particle size and are uniformly dispersed, thereby being more beneficial to improving the grinding effect when the cerium oxide dispersion is used as an abrasive for a planarization process.
In an embodiment of the present application, the cerium oxide dispersion has a solids content of 1 wt% to 5 wt%. In some embodiments, the cerium oxide dispersion has a solids content of 1 wt.%. In some embodiments, the cerium oxide dispersion has a solids content of 2 wt.%. In some embodiments, the ceria dispersion has a solids content of 3 wt%. In some embodiments, the cerium oxide dispersion has a solids content of 4 wt.%. In some embodiments, the cerium oxide dispersion has a solids content of 5 wt.%. Suitable solids content control, i.e. suitable content control of cerium oxide particles, is advantageous not only for preservation of the cerium oxide dispersion, but also for subsequent addition to the slurry system.
The cerium oxide dispersion liquid provided by the embodiment of the application can be used as an abrasive for preparing grinding liquid (namely polishing liquid), the abrasive is a colloidal nano cerium oxide abrasive with small size, rich defects and high activity, and the grinding liquid prepared by adopting the abrasive is used for flattening a dielectric layer (namely chemical-mechanical-polishing process), so that higher grinding removal rate and lower surface scratch can be obtained, and the grinding effect is improved.
In the prior art, the preparation method of the cerium oxide abrasive mainly comprises a calcination method, a hydrothermal method, a spray pyrolysis method and a sanding method; the preparation process of the calcination method is simple, the cost is low, the calcination method is suitable for expanded production, but the product particles are uneven and large; the product of the hydrothermal method has controllable morphology and particle size and good crystallinity, but the existing preparation process is complex and is carried out at high temperature and high pressure, thus being not beneficial to the expansion of production and having environmental hazard as a byproduct; the spray pyrolysis method has uniform and controllable product particles, is suitable for expanded production, has high product purity, but has high energy consumption and high cost in the preparation process, and has complex product morphology and larger particles; the sand grinding method has simple preparation process and is suitable for expanded production, but the sand grinding method takes large-particle solid as a raw material to carry out physical cutting, the appearance is uncontrollable, and the particle size of the product is larger. Therefore, the embodiment of the application provides a preparation method of cerium oxide dispersion liquid, which can realize the preparation of cerium oxide with smaller particle size and better grinding effect, has simpler process and is suitable for expanded production.
Specifically, the embodiment of the application provides a preparation method of cerium oxide dispersion liquid, which comprises the following steps:
Adding soluble cerium salt into organic alcohol or a mixture of organic alcohol and water to obtain a mixed solution, adding organic alkali into the mixed solution to form a precipitate in the mixed solution to obtain a precipitate mixture, removing supernatant in the precipitate mixture, and adding a first solvent to obtain cerium oxide dispersion; in the preparation process, a pH regulator is adopted to regulate the pH of the system, so that the pH of the cerium oxide dispersion liquid is 2.0-4.0; the cerium oxide dispersion liquid includes a first solvent and cerium oxide particles dispersed in the first solvent, wherein a signal peak position of electron spin resonance of the cerium oxide particles is less than or equal to 2.05.
According to the preparation method of the cerium oxide dispersion liquid, through selecting specific reaction raw materials and carrying out specific regulation and control on the pH value of a system, the preparation of colloidal cerium oxide with the signal peak position of electron spin resonance of cerium oxide particles smaller than or equal to 2.05 and smaller particle size can be realized, and the prepared colloidal cerium oxide can be used as an abrasive in the planarization process, so that the grinding removal rate is improved under the condition of not increasing the particle size of cerium oxide particles; the preparation method of the cerium oxide dispersion liquid provided by the embodiment of the application has the advantages of simple process and easiness in realizing industrial production.
In an embodiment of the present application, the above preparation process is carried out at a temperature of 25℃to 60 ℃. In some embodiments, the temperature is 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃. The temperature in the preparation process is controlled in a proper range, which is beneficial to preparing cerium oxide particles with improved grinding performance.
In an embodiment of the application, the organic base is added dropwise at a rate of 10mL/min to 40 mL/min. In some embodiments, the organic base is added dropwise at a rate of 10mL/min, 15mL/min, 20mL/min, 25mL/min, 30mL/min, 35mL/min, 40 mL/min. The organic base is controlled at a suitable dropping rate so that the nucleation rate of the cerium oxide is greater than the growth rate, thereby facilitating better control of the formation of cerium oxide particles having a smaller particle size.
In an embodiment of the present application, the soluble cerium salt may include one or more of cerium nitrate, cerium sulfate, ammonium cerium nitrate, cerium chloride, cerium acetate, cerium oxalate, and cerium acetylacetonate. The soluble cerium salt may provide a source of cerium for the reaction system.
In an embodiment of the present application, the organic alcohol includes monohydric alcohols having 1 to 10 carbon atoms. The organic alcohol may be, for example, methanol, ethanol, n-propanol, isopropanol, n-butanol, n-pentanol, isopentanol, or the like.
In an embodiment of the present application, the organic base may be one or more selected from ammonia, ethanolamine, diethanolamine, triethanolamine, imidazole, pyridine, pyrazole, diethylamine, and triethylamine alcohol amine.
In an embodiment of the present application, the pH adjuster includes nitric acid. Nitric acid is used as a pH regulator, so that the method is beneficial to being suitable for application scenes of dielectric layer planarization.
The embodiment of the application also provides a flattening composition, which comprises the cerium oxide dispersion liquid and the second solvent. The second solvent may be water in particular. The planarization composition can be used to planarize the dielectric layer by a combination of both chemical and mechanical actions. The planarization composition is a polishing liquid (i.e., a polishing liquid).
In embodiments of the present application, the planarization composition may further include an additive. The additives may be mainly betaine, glycine, proline, polyethylenimine, histidine, polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, lauryl betaine, citric acid betaine, cetyl sulfobetaine, tetradecyl sulfobetaine, thiobetaine 8, and thiobetaine 10. The additive can be added in proper amount according to actual needs.
In an embodiment of the present application, the pH of the planarization composition is from 4.0 to 7.0. In some embodiments of the present application, the pH of the planarization composition may be, for example, specifically 4.0, 5.0, 6.0, 7.0. The pH of the planarization composition is controlled within a range of 4.0 to 7.0, so that the adsorption of cerium oxide to the dielectric layer can be promoted, thereby promoting the improvement of the polishing effect.
The embodiment of the application also provides the cerium oxide dispersion liquid disclosed by the embodiment of the application or the application of the flattening composition disclosed by the embodiment of the application in flattening a dielectric layer.
In the embodiment of the present application, the dielectric layer may be a dielectric material layer commonly used in the field of electronic manufacturing, and may include, for example, a silicon oxide layer, a silicon nitride layer, a polysilicon layer, and the like.
The embodiment of the application also provides the cerium oxide dispersion liquid disclosed by the embodiment of the application or the application of the flattening composition disclosed by the embodiment of the application in glass flattening. The glass may be, for example, colorless optical glass, colored optical glass, laser glass, quartz optical glass, radiation-resistant glass, ultraviolet-infrared (high-transmittance, absorption) optical glass, fiber optical glass, acousto-optic glass, magneto-optic glass, photochromic glass, photomask glass, and the like.
The embodiment of the application also provides a flattening method, which adopts the flattening composition as the grinding fluid, so that the flattening composition contacts with the surface of the object to be flattened and relatively moves the object to be flattened. Taking an object to be planarized as a semiconductor structure (hereinafter referred to as a substrate) having a silicon dioxide dielectric layer as an example, the planarization method specifically includes: the planarization composition of the present embodiments is brought into contact with the silicon dioxide dielectric layer on the substrate surface and moves the silicon dioxide dielectric layer on the polished substrate surface relative to the substrate. According to the planarization method, the planarization composition is adopted for planarization treatment, so that the occurrence of surface scratch defects can be effectively reduced, and a higher polishing removal rate can be obtained, thereby improving the polishing effect.
As shown in fig. 1, in the process of the planarization method according to the embodiment of the present application, a polishing pad 102 is flatly attached to a polishing table 101, an object 103 to be planarized is hung upside down on a polishing head 104 (a surface to be polished of the object 103 to be planarized is in contact with the polishing head 104), and then is pressed against the polishing pad 102 rotating on the polishing table 101 with a certain pressure. When the planarization process is performed, the polishing head 104 starts rotating with the object 103 to be planarized, and the polishing table 101 also rotates at a certain speed. At the same time, the polishing liquid 105, i.e., the planarization composition, is added to the polishing pad 102 at a rate and spreads out with centrifugal force. The object 103 to be planarized is subjected to the dual action of chemistry and machinery to effect the removal of the silicon dioxide dielectric layer. And after the flattening process is finished, removing residual abrasive materials and organic matters on the surface of the substrate through a post-cleaning process.
The following examples are provided to further illustrate embodiments of the application.
Example 1
Adding about 1kg of cerium nitrate into enough absolute ethyl alcohol at 25 ℃ and stirring to obtain a mixed solution; dropwise adding an ammonia water solution into the mixed solution at a speed of 40mL/min until a precipitate is formed in the mixed solution to obtain a precipitate mixture; removing the supernatant except the precipitate in the precipitate mixture, and adding a certain amount of ultrapure water to form cerium oxide colloid, thus obtaining cerium oxide dispersion liquid; in the preparation process, a pH regulator is adopted to regulate the pH of the system, so that the pH of the cerium oxide dispersion liquid is 2.0-4.0; the resulting cerium oxide dispersion includes water and cerium oxide particles dispersed in the water.
The hydrated particle diameter d of the cerium oxide particles in the cerium oxide dispersion obtained in example 1 was measured by a dynamic light scattering DLS method; the signal peak position of the electron spin resonance ESR of the cerium oxide particles in the cerium oxide dispersion obtained in example 1 was measured using an electron spin resonance spectrometer; the cerium oxide dispersion obtained in example 1 was tested for the angle value of the X-ray diffraction angle 2θ corresponding to the (111) crystal plane of the cerium oxide particles using an X-ray diffractometer. The solid content of the cerium oxide dispersion obtained in example 1 was adjusted to 0.3%, and the average light transmittance of the cerium oxide dispersion at a solid content of 0.3% by weight was measured with a spectrophotometer for light having a wavelength of 190nm to 370nm and for light having a wavelength of 190nm to 320 nm. The test results are shown in Table 1.
TABLE 1
Example 2
About 1kg of cerium nitrate is added into enough isopropanol at 25 ℃ and stirred to obtain a mixed solution; dropwise adding a triethanolamine solution into the mixed solution at a speed of 30mL/min until a precipitate is formed in the mixed solution to obtain a precipitate mixture; removing the supernatant except the precipitate in the precipitate mixture, and adding a certain amount of ultrapure water to form cerium oxide colloid, thus obtaining cerium oxide dispersion liquid; in the preparation process, a pH regulator is adopted to regulate the pH of the system, so that the pH of the cerium oxide dispersion liquid is 2.0-4.0; the resulting cerium oxide dispersion includes water and cerium oxide particles dispersed in the water.
The hydrated particle diameter d of cerium oxide particles, the signal peak position of electron spin resonance ESR, and the angle value of the X-ray diffraction angle 2θ corresponding to the (111) crystal plane in the obtained cerium oxide dispersion were measured by the same method as in example 1; and measuring the average light transmittance of the resulting cerium oxide dispersion at a solid content of 0.3% by weight for light having a wavelength of 190nm to 370nm and the average light transmittance for light having a wavelength of 190nm to 320 nm. The results of the above test are shown in Table 2.
TABLE 2
Example 3
Adding about 1kg of cerium nitrate into sufficient n-butanol at 40 ℃ and stirring to obtain a mixed solution; dripping ethanolamine solution into the mixed solution at the speed of 20mL/min until a precipitate is formed in the mixed solution to obtain a precipitate mixture; removing the supernatant except the precipitate in the precipitate mixture, and adding a certain amount of ultrapure water to form cerium oxide colloid, thus obtaining cerium oxide dispersion liquid; in the preparation process, a pH regulator is adopted to regulate the pH of the system, so that the pH of the cerium oxide dispersion liquid is 2.0-4.0; the resulting cerium oxide dispersion includes water and cerium oxide particles dispersed in the water.
The hydrated particle diameter d of cerium oxide particles, the signal peak position of electron spin resonance ESR, and the angle value of the X-ray diffraction angle 2θ corresponding to the (111) crystal plane in the obtained cerium oxide dispersion were measured by the same method as in example 1; and measuring the average light transmittance of the resulting cerium oxide dispersion at a solid content of 0.3% by weight for light having a wavelength of 190nm to 370nm and the average light transmittance for light having a wavelength of 190nm to 320 nm. The results of the above test are shown in Table 3.
TABLE 3 Table 3
Example 4
Adding about 1kg of cerium nitrate into a sufficient amount of ethanol water mixture at 60 ℃ and stirring to obtain a mixed solution; dropwise adding an ammonia water solution into the mixed solution at a speed of 10mL/min until a precipitate is formed in the mixed solution to obtain a precipitate mixture; removing the supernatant except the precipitate in the precipitate mixture, and adding a certain amount of ultrapure water to form cerium oxide colloid, thus obtaining cerium oxide dispersion liquid; in the preparation process, a pH regulator is adopted to regulate the pH of the system, so that the pH of the cerium oxide dispersion liquid is 2.0-4.0; the resulting cerium oxide dispersion includes water and cerium oxide particles dispersed in the water.
The hydrated particle diameter d of cerium oxide particles, the signal peak position of electron spin resonance ESR, and the angle value of the X-ray diffraction angle 2θ corresponding to the (111) crystal plane in the obtained cerium oxide dispersion were measured by the same method as in example 1; and measuring the average light transmittance of the resulting cerium oxide dispersion at a solid content of 0.3% by weight for light having a wavelength of 190nm to 370nm and the average light transmittance for light having a wavelength of 190nm to 320 nm. The results of the above test are shown in Table 4.
TABLE 4 Table 4
Example 5
Adding about 1kg of cerium nitrate into sufficient n-amyl alcohol at 25 ℃ and stirring to obtain a mixed solution; dropwise adding an ammonia water solution into the mixed solution at a speed of 20mL/min until a precipitate is formed in the mixed solution to obtain a precipitate mixture; removing the supernatant except the precipitate in the precipitate mixture, and adding a certain amount of ultrapure water to form cerium oxide colloid, thus obtaining cerium oxide dispersion liquid; in the preparation process, a pH regulator is adopted to regulate the pH of the system, so that the pH of the cerium oxide dispersion liquid is 2.0-4.0; the resulting cerium oxide dispersion includes water and cerium oxide particles dispersed in the water.
Example 6
Adding about 1kg of cerium nitrate into enough isoamyl alcohol at the temperature of 25 ℃ and stirring to obtain a mixed solution; dropwise adding triethanolamine solution into the mixed solution at a speed of 25mL/min until a precipitate is formed in the mixed solution to obtain a precipitate mixture; removing the supernatant except the precipitate in the precipitate mixture, and adding a certain amount of ultrapure water to form cerium oxide colloid, thus obtaining cerium oxide dispersion liquid; in the preparation process, a pH regulator is adopted to regulate the pH of the system, so that the pH of the cerium oxide dispersion liquid is 2.0-4.0; the resulting cerium oxide dispersion includes water and cerium oxide particles dispersed in the water.
Example 7
About 1kg of cerium nitrate is added into sufficient n-propanol at 25 ℃ and stirred to obtain a mixed solution; dropwise adding an ammonia water solution into the mixed solution at a speed of 20mL/min until a precipitate is formed in the mixed solution to obtain a precipitate mixture; removing the supernatant except the precipitate in the precipitate mixture, and adding a certain amount of ultrapure water to form cerium oxide colloid, thus obtaining cerium oxide dispersion liquid; in the preparation process, a pH regulator is adopted to regulate the pH of the system, so that the pH of the cerium oxide dispersion liquid is 2.0-4.0; the resulting cerium oxide dispersion includes water and cerium oxide particles dispersed in the water.
Example 8
Adding about 1kg of cerium nitrate into sufficient n-butanol and water at 25 ℃ and stirring to obtain a mixed solution; dropwise adding an imidazole solution into the mixed solution at a speed of 25mL/min until a precipitate is formed in the mixed solution to obtain a precipitate mixture; removing the supernatant except the precipitate in the precipitate mixture, and adding a certain amount of ultrapure water to form cerium oxide colloid, thus obtaining cerium oxide dispersion liquid; in the preparation process, a pH regulator is adopted to regulate the pH of the system, so that the pH of the cerium oxide dispersion liquid is 2.0-4.0; the resulting cerium oxide dispersion includes water and cerium oxide particles dispersed in the water.
The hydrated particle diameter d of the cerium oxide particles in the cerium oxide dispersion liquid obtained in examples 5 to 8 was measured by a dynamic light scattering DLS method; the signal peak positions of the electron spin resonance ESR of the cerium oxide particles in the cerium oxide dispersions obtained in examples 5 to 8 were measured using an electron spin resonance spectrometer; the angle values of the X-ray diffraction angles 2θ corresponding to the (111) crystal planes of the cerium oxide particles in the cerium oxide dispersion obtained in examples 5 to 8 were measured using an X-ray diffractometer. The solid contents of the cerium oxide dispersions obtained in examples 5 to 8 were adjusted to 0.3%, respectively, and the average light transmittance of the cerium oxide dispersions at a solid content of 0.3% by weight for light having a wavelength of 190nm to 370nm and the average light transmittance for light having a wavelength of 190nm to 320nm were measured using a spectrophotometer. The results of the above test are shown in Table 5.
TABLE 5
The cerium oxide dispersions of examples 1 to 8 of the present application were formulated into a planarization composition having a solid content of 0.3% using solvent water, and the pH was adjusted to 5.0. Two kinds of cerium oxide particle dispersions commercially available were simultaneously used as comparative example 1 and comparative example 2, and a leveling composition having a solid content of 0.3% was prepared using solvent water in the same manner as in examples 1 to 8, and the pH was adjusted to 5.0. In comparative example 1, the cerium oxide particles had a hydrated particle diameter of 50nm, no electron spin resonance signal peak, and an angle value of the X-ray diffraction angle 2θ corresponding to the (111) crystal plane was 28.5. In comparative example 2, the cerium oxide particles had a hydrated particle diameter of 10nm, no electron spin resonance signal peak, and an angle value of the X-ray diffraction angle 2θ corresponding to the (111) crystal plane was 28.6.
The planarization compositions obtained in examples 1 to 8, and comparative examples 1 and 2 were used for planarization treatment of a silicon dioxide dielectric layer, and the silicon dioxide removal rate results thereof are shown in table 6.
TABLE 6
From the results of table 6, it can be seen that the silica removal rates of the planarization compositions prepared using the cerium oxide dispersions of examples 1 to 8 of the present application are significantly improved over those of the planarization compositions prepared using the existing commercially available cerium oxide particle dispersions of comparative examples 1 and 2. The cerium oxide dispersion liquid provided by the embodiment of the application can improve the silicon dioxide removal rate under the condition that cerium oxide particles have smaller particle size, so that the planarization rate can be improved while the occurrence of surface scratch defects is reduced, and finally the planarization effect of a dielectric medium is improved.
It should be understood that the first, second, and various numerical numbers referred to herein are merely descriptive convenience and are not intended to limit the scope of the application.
In the present application, "and/or" describing the association relationship of the association object means that there may be three relationships, for example, a and/or B may mean: a alone, a and B together, and B alone, wherein a, B may be singular or plural. The character "/" generally indicates that the context-dependent object is an "or" relationship.
In the present application, "at least one" means one or more, and "a plurality" means two or more. "at least one of" or the like means any combination of these items, including any combination of single item(s) or plural items(s). For example, "at least one (individual) of a, b, or c," or "at least one (individual) of a, b, and c," may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, c may be single or multiple, respectively.
It should be understood that, in various embodiments of the present application, the sequence number of each process described above does not mean that the execution sequence of some or all of the steps may be executed in parallel or executed sequentially, and the execution sequence of each process should be determined by its functions and internal logic, and should not constitute any limitation on the implementation process of the embodiments of the present application.
Claims (23)
1. A dispersion liquid comprising a first solvent and cerium oxide particles dispersed in the first solvent, wherein the cerium oxide particles have an electron spin resonance signal peak, and the peak position of the electron spin resonance signal peak is 2.05 or less.
2. The dispersion according to claim 1, wherein the cerium oxide particles have an X-ray diffraction angle 2Θ corresponding to the (111) crystal plane of less than or equal to 28.6 °.
3. The dispersion according to claim 1 or 2, wherein the pH of the dispersion is in the range of 2.0-4.0.
4. A dispersion according to claim 3, wherein the pH of the dispersion is in the range of 2.0 to 3.0.
5. The dispersion liquid according to any one of claims 1 to 4, wherein the hydrated particle diameter of the cerium oxide particles is nano-scale.
6. The dispersion of claim 5, wherein the cerium oxide particles have a hydrated particle size of less than or equal to 50nm.
7. The dispersion according to any one of claims 1 to 6, wherein the dispersion has an average light transmittance of less than 5% for light having a wavelength of 190nm to 370nm when the solids content is adjusted to 0.3% by weight.
8. The dispersion of claim 7, wherein the dispersion has an average light transmittance of less than or equal to 2.5% for light having a wavelength of 190nm to 370nm when the solids content is adjusted to 0.3% by weight.
9. The dispersion according to any one of claims 1 to 8, wherein the dispersion has an average light transmittance of less than 0.01% for light having a wavelength of 190nm to 320nm when the solids content is adjusted to 0.3% by weight.
10. The dispersion of claim 9, wherein the dispersion has an average light transmittance of less than or equal to 0.005% for light having a wavelength of 190nm to 320nm when the solids content is adjusted to 0.3% by weight.
11. The dispersion according to any one of claims 1 to 10, wherein the solids content of the dispersion is from 1% to 5% by weight.
12. A method for preparing a dispersion, comprising:
Adding soluble cerium salt into organic alcohol or a mixture of organic alcohol and water to obtain a mixed solution, adding organic alkali into the mixed solution to form a precipitate in the mixed solution to obtain a precipitate mixture, removing supernatant in the precipitate mixture, and adding a first solvent to obtain a dispersion; in the preparation process, a pH regulator is adopted to regulate the pH of the system, so that the pH of the dispersion liquid is 2.0-4.0; the dispersion liquid comprises a first solvent and cerium oxide particles dispersed in the first solvent, wherein the signal peak position of electron spin resonance of the cerium oxide particles is less than or equal to 2.05.
13. The method of preparing according to claim 12, wherein the soluble cerium salt comprises one or more of cerium nitrate, cerium sulfate, ammonium cerium nitrate, cerium chloride, cerium acetate, cerium oxalate, cerium acetylacetonate.
14. The method of claim 12 or 13, wherein the organic alcohol comprises a monohydric alcohol having 1 to 10 carbon atoms.
15. The method of any one of claims 12-14, wherein the organic base comprises one or more of ammonia, ethanolamine, diethanolamine, triethanolamine, imidazole, pyridine, pyrazole, diethylamine, triethylamine.
16. The method of any one of claims 12-15, wherein the pH adjuster comprises nitric acid.
17. A levelling composition comprising the dispersion of any one of claims 1 to 11 and a second solvent.
18. The planarization composition of claim 17, it is characterized in that the method comprises the steps of, the planarization composition also includes an additive.
19. The planarization composition of claim 17 or 18, wherein the planarization composition has a pH of 4.0 to 7.0.
20. Use of the dispersion according to any one of claims 1 to 11 or the planarization composition according to any one of claims 17 to 19 for planarizing a dielectric layer.
21. The use of claim 20, wherein the dielectric layer comprises a silicon dioxide layer, a silicon nitride layer, a polysilicon layer.
22. Use of the dispersion according to any one of claims 1 to 11 or the flattening composition according to any one of claims 17 to 19 for glass flattening.
23. A planarization method, characterized in that the planarization composition of any one of claims 17 to 19 is brought into contact with the surface of an object to be planarized and relatively moves the object to be planarized.
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