WO2018216218A1 - Dispersion dans un liquide contenant des nanobulles de particules fines d'un oxyde inorganique, abrasif la contenant, et procédés de production associés - Google Patents
Dispersion dans un liquide contenant des nanobulles de particules fines d'un oxyde inorganique, abrasif la contenant, et procédés de production associés Download PDFInfo
- Publication number
- WO2018216218A1 WO2018216218A1 PCT/JP2017/019791 JP2017019791W WO2018216218A1 WO 2018216218 A1 WO2018216218 A1 WO 2018216218A1 JP 2017019791 W JP2017019791 W JP 2017019791W WO 2018216218 A1 WO2018216218 A1 WO 2018216218A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- inorganic oxide
- oxide fine
- particle dispersion
- fine particle
- nanobubble
- Prior art date
Links
- 239000010419 fine particle Substances 0.000 title claims abstract description 170
- 239000002101 nanobubble Substances 0.000 title claims abstract description 126
- 239000006185 dispersion Substances 0.000 title claims abstract description 118
- 229910052809 inorganic oxide Inorganic materials 0.000 title claims abstract description 110
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 239000007788 liquid Substances 0.000 title abstract description 29
- 239000002245 particle Substances 0.000 claims abstract description 52
- 239000007864 aqueous solution Substances 0.000 claims abstract description 35
- 239000000243 solution Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims description 19
- 230000001590 oxidative effect Effects 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229910052684 Cerium Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 87
- 239000000377 silicon dioxide Substances 0.000 description 43
- 238000005498 polishing Methods 0.000 description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 18
- 239000007787 solid Substances 0.000 description 18
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 14
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 14
- 238000003756 stirring Methods 0.000 description 14
- 239000004065 semiconductor Substances 0.000 description 9
- 229910004298 SiO 2 Inorganic materials 0.000 description 8
- 239000011362 coarse particle Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 241000233866 Fungi Species 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 241000195493 Cryptophyta Species 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 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 description 4
- 238000000691 measurement method Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 238000007517 polishing process Methods 0.000 description 4
- 230000002829 reductive effect Effects 0.000 description 4
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 239000002612 dispersion medium Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 230000000366 juvenile effect Effects 0.000 description 3
- 229910052746 lanthanum Inorganic materials 0.000 description 3
- 244000005700 microbiome Species 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- WRAGBEWQGHCDDU-UHFFFAOYSA-M C([O-])([O-])=O.[NH4+].[Zr+] Chemical compound C([O-])([O-])=O.[NH4+].[Zr+] WRAGBEWQGHCDDU-UHFFFAOYSA-M 0.000 description 2
- 235000002597 Solanum melongena Nutrition 0.000 description 2
- 239000008186 active pharmaceutical agent Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052790 beryllium Inorganic materials 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 230000009172 bursting Effects 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- 238000003703 image analysis method Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 230000002147 killing effect Effects 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000001766 physiological effect Effects 0.000 description 2
- 230000000644 propagated effect Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 229910052712 strontium Inorganic materials 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910052727 yttrium Inorganic materials 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- WSMQKESQZFQMFW-UHFFFAOYSA-N 5-methyl-pyrazole-3-carboxylic acid Chemical compound CC1=CC(C(O)=O)=NN1 WSMQKESQZFQMFW-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002353 algacidal effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000013480 data collection Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000035784 germination Effects 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 150000002391 heterocyclic compounds Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000001418 larval effect Effects 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000006179 pH buffering agent Substances 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000002062 proliferating effect Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
- C01F17/224—Oxides or hydroxides of lanthanides
- C01F17/235—Cerium oxides or hydroxides
-
- 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
-
- 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
Definitions
- the present invention relates to a method for producing a nanobubble-containing inorganic oxide fine particle dispersion in which the inorganic oxide fine particle dispersion contains nanobubbles (microbubbles), and a nanobubble-containing inorganic oxide fine particle dispersion obtained by the production method. It is.
- the present invention also provides a method for producing an abrasive (polishing slurry) containing the nanobubble-containing inorganic oxide fine particle dispersion, and an abrasive containing an nanobubble-containing inorganic oxide fine particle dispersion obtained by the production method (for polishing). Slurry).
- the surface state affects the semiconductor characteristics, and therefore, it is required to polish the surfaces and end faces of these components with extremely high accuracy.
- a polishing method for such a member after performing a relatively rough primary polishing process, and then performing a precise secondary polishing process, a smooth surface or a highly accurate surface with few scratches such as scratches can be obtained. The way to get done.
- the following method has been proposed as an abrasive used for such secondary polishing as final polishing.
- Patent Document 1 discloses a silica sol in which silica fine particles are dispersed in a dispersion medium, and the mode particle diameter in the particle size distribution of the silica fine particles is in the range of 5 to 100 nm, and 1) mode particles The proportion of silica fine particles exceeding the diameter is in the range of 0.1 to 30% by volume with respect to the total silica fine particles. 2) The particle size variation coefficient in the particle size distribution below the mode particle size is 8 to 70%.
- a polishing silica sol characterized by satisfying the condition that it is in the range of. And, according to such a silica sol for polishing, it is described that it is applied to a polishing application, and generation of linear traces, scratches and the like is suppressed, and an excellent polishing rate is continuously exhibited.
- inorganic oxide fine particle dispersions in which inorganic oxide fine particles such as silica fine particles are dispersed in a dispersion medium are suitable for transporting operations and handling in various processes unless there is a particular problem. ing.
- the polishing treatment is often performed in an open system, and when the polishing liquid is prepared, the surrounding environment changes (temperature, humidity, etc.) and stirring in the tank.
- foreign matters such as dry matter and microgel due to partial concentration are generated due to fluctuations in the surface of the polishing liquid due to the liquid and splashed liquid. It has been broken.
- polishing liquid is circulated again and used as necessary, Due to changes in the level of the circulating tank due to the consumption of the polishing liquid, and fluctuations in the liquid level due to the falling of the polishing liquid from the return line of the circulating liquid, generation of microgel due to scale generation and concentration of the polishing liquid, and agglomeration It often leads to the production of things. Such foreign matters are hard and large foreign matters can be removed to some extent by microfiltration, but it is particularly difficult to completely remove fine microgels that are particularly flexible.
- the inorganic oxide fine particle dispersion is also used in the preparation process and the polishing process, in the surrounding environment (temperature, humidity, etc.) and fluctuations in the liquid level of the polishing liquid due to stirring in the tank, In many cases, non-sedimentable fine particles or microgels are generated by the scattering liquid or the like. In the case where the inorganic oxide fine particle dispersion is applied for polishing, the non-sedimentable fine particles or microgel are further aggregated into coarse particles, and the filtration treatment is performed before the inorganic oxide fine particle dispersion is used for polishing. It has been known that the filterability tends to be lowered.
- an object of the present invention is to provide a nanobubble-containing inorganic oxide fine particle dispersion excellent in concentration stability in a process used as an abrasive, an abrasive containing the same, and a method for producing the same.
- the present invention reduces the microgel by suppressing the generation of coarse particles by crushing and dispersing the microgel present in the inorganic oxide fine particle dispersion such as silica fine particle dispersion due to the bursting effect of the nanobubbles. By doing so, concentration stability and filterability improvement are achieved.
- the present invention includes the following (1) to (9).
- An inorganic oxide fine particle dispersion containing fine particles containing Ce having an average particle size of 1 to 500 nm, and an average bubble size of 50 to 500 nm, and at least one selected from the group consisting of N 2 and H 2 A method of producing a nanobubble-containing inorganic oxide fine particle dispersion comprising a step of mixing a solution containing a nanobubble aqueous solution containing nanobubbles, which is a non-oxidizing gas, while maintaining the solution at 5 to 80 ° C.
- An abrasive comprising the nanobubble-containing inorganic oxide fine particle dispersion described in (5) above.
- the average particle diameter is 1 to 500 nm
- the average bubble diameter is 50 to 500 nm to the inorganic oxide fine particle dispersion containing fine particles containing Ce, and N 2 and H
- a method for filtering an inorganic oxide fine particle dispersion comprising adding an aqueous nanobubble solution containing nanobubbles that are at least one non-oxidizing gas selected from the group consisting of 2 , mixing, and then filtering.
- the average particle size is 1 to 500 nm
- the average bubble size is 50 to 500 nm inside the inorganic oxide fine particle dispersion containing fine particles containing Ce, and N 2
- the nanobubble-containing inorganic oxide fine particle dispersion that is excellent in concentration stability and filterability and suppresses a decrease in workability even if solid content increases due to concentration or the like in the step of using as an abrasive,
- polishing agent containing it and those manufacturing methods can be provided.
- the present invention maintains a solution containing an inorganic oxide fine particle dispersion containing fine particles having an average particle size of 1 to 500 nm and a nanobubble aqueous solution containing nanobubbles having an average bubble size of 50 to 500 nm at 5 to 80 ° C.
- a method for producing a nanobubble-containing inorganic oxide fine particle dispersion comprising a mixing step.
- such a method for producing a nanobubble-containing inorganic oxide fine particle dispersion is also referred to as “the production method of the present invention”.
- an inorganic oxide fine particle dispersion and a nanobubble aqueous solution are prepared.
- the inorganic oxide fine particle dispersion is obtained by dispersing inorganic oxide fine particles (sometimes simply referred to as fine particles) having an average particle diameter of 1 to 500 nm in a solvent.
- the average particle size of the inorganic oxide fine particles means a value calculated from a measurement result by an image analysis method.
- the inorganic oxide fine particles include, for example, Si, Al, B, Mg, Ca, Ba, Mo, Zr, Ga, Be, Sr, Y, La, Ce, Sn, Fe, Zn, Mn, C, H, and Ti.
- the main component is an oxide containing at least one element selected from the group consisting of:
- the inorganic oxide fine particles are more preferably substantially composed of such an oxide.
- the inorganic oxide fine particles may be inorganic composite oxide fine particles.
- the “main component” has a content of 50% by mass or more (that is, Si, Al, B, Mg, Ca, Ba, Mo, Zr, Ga, Be, Sr, inorganic oxide fine particles are included).
- Y, La, Ce, Sn, Fe, Zn, Mn, C, H, and Ti oxide total content is preferably 50% by mass or more, more preferably 60% by mass or more, 80 It is more preferably at least mass%, more preferably at least 90 mass%, and even more preferably at least 95 mass%.
- “substantially” means that impurities mixed in from the raw materials and the manufacturing process can be included. In the following, the terms “main component” and “substantially” are used in this sense unless otherwise specified.
- a non-oxidizing gas such as N 2 or H 2 as nanobubbles. preferable.
- a non-oxidizing gas as nanobubbles even when the inorganic oxide fine particles form an interstitial solid solution due to the presence of heteroelements and oxygen vacancies increase.
- the inorganic oxide fine particles contain Ce and further contain a hetero element such as Si, C, N, La and Zr.
- the average particle diameter of the inorganic oxide fine particles is 500 nm or less, preferably 300 nm or less, more preferably 200 nm or less, and even more preferably 100 nm or less.
- the average particle size is 1 nm or more, and preferably 5 nm or more.
- the solvent in which the inorganic oxide fine particles are dispersed is not particularly limited, but is preferably water (including ion-exchanged water and pure water).
- the aqueous nanobubble solution contains nanobubbles having an average bubble diameter of 50 to 500 nm. Nano bubbles are fine bubbles having a bubble diameter of 500 nm or less.
- the bubble diameter is preferably 400 nm or less, and more preferably 350 nm or less.
- the bubble diameter is 50 nm or more, and more preferably 70 nm or more.
- the average bubble diameter and the number of bubbles in nanobubbles are measured using the nanoparticle tracking analysis method for the Brownian movement speed of bubbles in the liquid.
- the type of gas contained in the nanobubble is not particularly limited as long as the effect of crushing the microgel by bursting of the nanobubble can be exerted, but usually composed of N 2 , H 2 and O 2. It is preferable to consist essentially of at least one selected from the group.
- the inorganic oxide fine particles are silica fine particles
- the nanobubbles are preferably composed of N 2 and / or O 2 .
- the inorganic oxide fine particles are oxide fine particles or complex oxide fine particles containing Ce such as ceria
- the nanobubbles are preferably a non-oxidizing gas.
- the nanobubble aqueous solution preferably contains 1.0 ⁇ 10 5 / mL or more nanobubbles, more preferably 1.1 ⁇ 10 5 / mL or more nanobubbles, and 1.0 ⁇ 10 8 / mL. It is more preferable to include the above nanobubbles, and it is further preferable to include 1.1 ⁇ 10 8 / mL or more nanobubbles.
- the number of nanobubbles is preferably 1000 ⁇ 10 8 pieces / mL or less, more preferably 500 ⁇ 10 8 pieces / mL or less, and further preferably 100 ⁇ 10 8 pieces / mL or less.
- the method for generating microbubbles is not particularly limited, and a conventionally known method can be used.
- a swirling flow type a static mixer type, an ejector type, a venturi type, a pressure dissolution type, a pore type, a rotary type, an ultrasonic type, a vapor condensation type, an electrolysis type and the like can be mentioned.
- the solution containing the above inorganic oxide fine particle dispersion liquid and nanobubble aqueous solution is obtained.
- This solution can be obtained by adding one to the other, but can also be obtained by generating nanobubbles inside the inorganic oxide fine particle dispersion.
- the method for generating nanobubbles inside the inorganic oxide fine particle dispersion is not particularly limited, and the above-described conventionally known methods can be used.
- the nanobubble containing inorganic oxide fine particle dispersion liquid which is excellent in concentration stability in the process used as an abrasive
- the temperature at which the solution containing the inorganic oxide fine particle dispersion and the nanobubble aqueous solution is maintained is 5 to 80 ° C., preferably 50 ° C. or less, and more preferably 30 ° C. or less.
- the mixing means is not particularly limited, and mixing by stirring is preferable. Although there is no special restriction
- the nanobubble-containing inorganic oxide fine particle dispersion obtained in this way is preferably used as an abrasive used for final polishing (secondary polishing), which is one of the processes for manufacturing semiconductor devices such as semiconductor substrates and wiring substrates. be able to.
- the nanobubble-containing inorganic oxide fine particle dispersion can be used as a polishing agent as it is, but as an additive, for example, a group consisting of conventionally known polishing accelerators, surfactants, heterocyclic compounds, pH adjusting agents and pH buffering agents. One or more selected from more may be included.
- the amount of microgel is small, since it is possible to improve the production efficiency if filtration of the abrasive can be completed in a short time.
- the nanobubble-containing inorganic oxide fine particle dispersion of the present invention is used as an abrasive, not only the filtration rate is very fast, but also the concentration stability is excellent.
- the inventor presumes that the reason why the filtration speed is fast and the concentration stability is improved is that the microgel is dispersed by the shock wave generated when the nanobubbles disappear. If the microgel disappears by being dispersed, coarse particles are further reduced, and it is considered that the surface accuracy of the polished surface is improved (reduction of scratches and the like). Furthermore, an improvement in the polishing rate is also observed.
- the present invention is a nanobubble-containing inorganic oxide fine particle dispersion produced by the production method of the present invention as described above and an abrasive containing the same.
- such a nanobubble-containing inorganic oxide fine particle dispersion and an abrasive containing the same are preferably maintained while holding a solution containing a specific inorganic oxide fine particle dispersion and a specific nanobubble aqueous solution at a specific temperature (preferably Is a product obtained by a production method comprising a step of mixing for a specific time.
- a specific temperature preferably Is a product obtained by a production method comprising a step of mixing for a specific time.
- the nanobubble-containing inorganic oxide fine particle dispersion of the present invention suppresses germination, generation and growth of larvae and juveniles of molds, fungi and algae in the dispersion due to the presence of nanobubbles in the dispersion ⁇ Can be killed.
- These organisms of several microns or less should be called nano-organisms, and are difficult to mechanically remove by ordinary filtration or the like, and can easily fly from the air. For this reason, they are killed with drugs, but it is inevitable that the substance itself is organic and remains as a source of contamination.
- nano-bubbles of several microns that are generally present in liquids are known to have killing, sterilizing, or algicidal effects on molds, fungi, and algae grown and propagated in liquids.
- nanobubbles of several microns are added to the solution after these microorganisms have propagated, the growth can be stopped, but a large amount of microorganism remains, and even if these dead bodies are filtered off, they remain on the filter surface. Breed on the dead carcass.
- nanobubbles of several microns have a life of several days or less, they are not durable and have little effect on spores that have passed through the filter or nano organisms that have come through the air.
- the chemicals added for the killing of nano-organisms or the remains of microorganisms remaining as foreign substances may affect the performance of the semiconductor.
- nanobubbles of several microns or less are added to the inorganic fine particle dispersion before the growth of fungi, fungi or algae sufficiently in the dispersion, the nanobubbles exist for several months or more. Can be destroyed at the pre-growth spore or larvae and juvenile stages.
- the inorganic oxide fine particle dispersion containing fine particles containing Ce, molds, fungi and algae are in the spore or larval and juvenile stages or earlier. It is preferred to use the dispersion containing the stages as raw material.
- the destruction mechanism of spores or larvae caused by nanobubbles of several microns or less occurs due to the phenomenon that the bubbles shrink and collapse over time due to the self-pressurization effect (hot spot phenomenon), destroying water molecules. These free radicals are thought to inhibit their physiological activities by breaking the molecular bonds on the outer surface of the spores, larvae and juveniles.
- the term “larvae” and “juvenile” used here are not strict terms. They are physiological activities in the pre-growth stage where the former is animal and the latter is capable of exerting a proliferative function in plant-based organisms. Used as a general term for living organisms.
- the specific polishing effect of Ce on silica is generally accepted by researchers such as academic societies as Ce 3+ on the surface of tetravalent ceria particles reacts specifically with silica. If this is correct, it is preferable that the ceria-based abrasive dispersion medium does not contain oxidizing substances.
- the present invention suppresses ceria oxidation and suppresses biological activity of nano-sized organisms, thereby suppressing substrate residual organic matter in the abrasive dispersion and polishing slurry. Can prevent contamination of the base.
- the average particle diameter of the inorganic oxide fine particles was measured by an image analysis method. Specifically, inorganic oxide fine particles are shown in a photograph projection view obtained by photographing a sample inorganic oxide fine particle dispersion at a magnification of 250,000 times with a transmission electron microscope (H-800, manufactured by Hitachi, Ltd.). The longest diameter is taken as the major axis, the length is measured, and the value is taken as the major diameter (DL).
- a point that bisects the major axis on the major axis is determined, two points where a straight line perpendicular to the major axis intersects the outer edge of the fine particle are obtained, and a distance between the two points is measured to obtain a minor axis (DS).
- the simple average value of the short diameter (DS) and the long diameter (DL) is defined as the particle diameter of the fine particles. In this way, the particle diameter was determined for any 500 fine particles, and the average value thereof was taken as the average particle diameter of the inorganic oxide fine particles.
- the average bubble diameter of the nanobubbles was measured using the nanoparticle 4 tracking analysis method for the Brownian movement speed of the bubbles in the liquid. Specifically, about 20 mL of a measurement sample (nanobubble-containing inorganic oxide fine particle dispersion) was injected while being sucked into a measuring instrument (“Nanosite NS300” manufactured by Malvern) and measured by a nanoparticle tracking analysis method.
- a measurement sample nanobubble-containing inorganic oxide fine particle dispersion
- ⁇ Reference Example 1 500 g of a silica fine particle dispersion (solid content concentration 5 mass%) in which silica fine particles having an average particle diameter of 3 nm are dispersed in water is prepared, and the temperature is maintained at 20 ° C. 500 g of an aqueous solution of nanobubbles containing 1 ⁇ 10 8 / ml N 2 was added. Then, the mixture was stirred for 1 hour while maintaining the same temperature to obtain a nanobubble-containing inorganic oxide fine particle dispersion. The obtained nanobubble-containing inorganic oxide fine particle dispersion was concentrated according to the concentration stability measurement method, and the concentration stability was evaluated. Table 1 shows the processing conditions and the measurement results.
- the filtration rate when the obtained nanobubble-containing inorganic oxide fine particle dispersion was filtered through a filtration filter (filter diameter: 0.5 ⁇ m) at a filtration pressure of 1 mPa was 35 g / min.
- the number of coarse particles having a particle diameter of 0.51 ⁇ m or more was measured using an Accusizer 780APS manufactured by PSS for the nanobubble-containing inorganic oxide fine particle dispersion that passed through the filter, and found to be 200,000 particles / ml.
- ⁇ Reference Example 2 500 g of a silica fine particle dispersion (solid content concentration: 40% by mass) in which silica fine particles having an average particle diameter of 80 nm are dispersed in water is prepared, and the temperature is maintained at 20 ° C. 500 g of an aqueous solution of nanobubbles containing 1 ⁇ 10 8 / ml N 2 was added. Then, after stirring for 2 hours while maintaining the same temperature, the obtained inorganic oxide fine particle dispersion was concentrated according to the concentration stability measurement method, and the concentration stability was evaluated. Table 1 shows the processing conditions and the measurement results.
- ⁇ Reference Example 5 500 g of a silica fine particle dispersion (solid content concentration 48 mass%) in which silica fine particles having an average particle diameter of 250 nm are dispersed in water is prepared, and the temperature is maintained at 5 ° C. 500 g of an aqueous solution of nanobubbles containing N 2 at 0 ⁇ 10 8 pieces / ml was added. Then, after stirring for 1.5 hours while maintaining the same temperature, the obtained solution was concentrated in the same manner as in Reference Example 1. Table 1 shows the processing conditions and the results.
- ⁇ Reference Example 7> Maintaining the pH of a silica fine particle dispersion (solid content concentration: 5% by mass) in which silica fine particles having an average particle diameter of 17 nm are dispersed in water at 9 and maintaining the temperature at 80 ° C., an aqueous solution of zirconium ammonium carbonate (converted to zirconia) Concentration: 5% by mass) was added over 5 hours.
- Example 1 500 g of a ceria fine particle dispersion (solid content concentration 20% by mass) in which ceria fine particles having an average particle diameter of 20 nm are dispersed in water is prepared, the temperature is maintained at 30 ° C., and 15% of the average bubble diameter is 290 nm. 500 g of a nanobubble aqueous solution containing ⁇ 10 8 / ml N 2 was added. Then, after stirring for 60 hours while maintaining a temperature of 30 ° C., the obtained solution was concentrated in the same manner as in Reference Example 1. Table 1 shows the processing conditions and the results.
- the filtration rate when the obtained nanobubble-containing inorganic oxide fine particle dispersion was filtered through a filtration filter (filter diameter: 0.5 ⁇ m) at a filtration pressure of 1 mPa as in Reference Example 1 was 10 g / min. there were.
- the number of coarse particles having a particle diameter of 0.51 ⁇ m or more was measured using an Accusizer 780APS manufactured by PSS for the nanobubble-containing inorganic oxide fine particle dispersion that passed through the filter, and the result was 600,000 particles / ml.
- ⁇ Comparative Example 5> 500 g of a silica / ceria fine particle dispersion in which silica / zirconia fine particles (SiO 2 / ZrO 2 mass ratio 75/25, solid concentration 20 mass%) having an average particle diameter of 20 nm are dispersed in water is prepared, and the temperature is 20 Held at 0C. And it concentrated similarly to the reference example 7, without adding nanobubble aqueous solution. Table 1 shows the processing conditions and the results.
- the concentration stability has a correlation with the particle size (average particle size) of the inorganic oxide fine particles, so the relationship between the average particle size and the concentration stability is shown in the graph (FIG. 1). From the graph of FIG. 1, for example, in the case of Reference Example 3, it can be seen that the concentration stability is superior to Comparative Example 1 or Comparative Example 2 in which the average particle diameter of the silica fine particles is the same. In addition, it can be seen that Reference Example 2 is superior in concentration stability as compared with Comparative Example 3 in which the average particle diameter of the silica fine particles is the same.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
La présente invention aborde le problème consistant à fournir un procédé de production d'une dispersion dans un liquide contenant des nanobulles de particules fines d'un oxyde inorganique, qui présente une excellente stabilité de la concentration dans un procédé utilisant la dispersion dans un liquide en tant qu'abrasif. Ce problème est résolu par un procédé de production d'une dispersion dans un liquide contenant des nanobulles de particules fines d'un oxyde inorganique, le procédé comprenant une étape de mélange d'une solution qui contient : une dispersion dans un liquide de particules fines d'un oxyde inorganique contenant des particules fines ayant une granulométrie moyenne de 1 à 500 nm ; et une solution aqueuse de nanobulles contenant des nanobulles ayant un diamètre moyen de bulle de 50 à 500 nm, la solution étant maintenue à 5 à 80 °C.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/JP2017/019791 WO2018216218A1 (fr) | 2017-05-26 | 2017-05-26 | Dispersion dans un liquide contenant des nanobulles de particules fines d'un oxyde inorganique, abrasif la contenant, et procédés de production associés |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PCT/JP2017/019791 WO2018216218A1 (fr) | 2017-05-26 | 2017-05-26 | Dispersion dans un liquide contenant des nanobulles de particules fines d'un oxyde inorganique, abrasif la contenant, et procédés de production associés |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2018216218A1 true WO2018216218A1 (fr) | 2018-11-29 |
Family
ID=64396456
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2017/019791 WO2018216218A1 (fr) | 2017-05-26 | 2017-05-26 | Dispersion dans un liquide contenant des nanobulles de particules fines d'un oxyde inorganique, abrasif la contenant, et procédés de production associés |
Country Status (1)
Country | Link |
---|---|
WO (1) | WO2018216218A1 (fr) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11505717B2 (en) | 2017-06-01 | 2022-11-22 | Jgc Catalysts And Chemicals Ltd. | Nanobubble-containing inorganic oxide fine particle and abrasive containing same |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2008235357A (ja) * | 2007-03-16 | 2008-10-02 | Toshiba Corp | 化学的機械的研磨方法および半導体装置の製造方法 |
JP2009111095A (ja) * | 2007-10-29 | 2009-05-21 | Covalent Materials Corp | ウェーハラッピング方法 |
JP2009111094A (ja) * | 2007-10-29 | 2009-05-21 | Covalent Materials Corp | ウェーハ鏡面研磨方法 |
JP2010042338A (ja) * | 2008-08-11 | 2010-02-25 | Aura Tec:Kk | 液中の粒子の浮上分離方法およびその装置 |
JP2011005584A (ja) * | 2009-06-25 | 2011-01-13 | Olympus Corp | 光学素子の研削研磨装置および光学素子の研削研磨方法ならびに光学素子の製造方法 |
WO2015064159A1 (fr) * | 2013-10-31 | 2015-05-07 | 日之出産業株式会社 | Procédé de formation de micro-bulles, et dispositif de formation de micro-bulles |
JP2015186838A (ja) * | 2014-03-14 | 2015-10-29 | 不二越機械工業株式会社 | ワーク研磨方法およびワーク研磨装置 |
JP6141482B1 (ja) * | 2016-03-28 | 2017-06-07 | 日揮触媒化成株式会社 | ナノバブル含有無機酸化物微粒子分散液、それを含む研磨剤およびそれらの製造方法 |
-
2017
- 2017-05-26 WO PCT/JP2017/019791 patent/WO2018216218A1/fr active Application Filing
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2008235357A (ja) * | 2007-03-16 | 2008-10-02 | Toshiba Corp | 化学的機械的研磨方法および半導体装置の製造方法 |
JP2009111095A (ja) * | 2007-10-29 | 2009-05-21 | Covalent Materials Corp | ウェーハラッピング方法 |
JP2009111094A (ja) * | 2007-10-29 | 2009-05-21 | Covalent Materials Corp | ウェーハ鏡面研磨方法 |
JP2010042338A (ja) * | 2008-08-11 | 2010-02-25 | Aura Tec:Kk | 液中の粒子の浮上分離方法およびその装置 |
JP2011005584A (ja) * | 2009-06-25 | 2011-01-13 | Olympus Corp | 光学素子の研削研磨装置および光学素子の研削研磨方法ならびに光学素子の製造方法 |
WO2015064159A1 (fr) * | 2013-10-31 | 2015-05-07 | 日之出産業株式会社 | Procédé de formation de micro-bulles, et dispositif de formation de micro-bulles |
JP2015186838A (ja) * | 2014-03-14 | 2015-10-29 | 不二越機械工業株式会社 | ワーク研磨方法およびワーク研磨装置 |
JP6141482B1 (ja) * | 2016-03-28 | 2017-06-07 | 日揮触媒化成株式会社 | ナノバブル含有無機酸化物微粒子分散液、それを含む研磨剤およびそれらの製造方法 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11505717B2 (en) | 2017-06-01 | 2022-11-22 | Jgc Catalysts And Chemicals Ltd. | Nanobubble-containing inorganic oxide fine particle and abrasive containing same |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Rouxel et al. | Dispersion of nanoparticles: From organic solvents to polymer solutions | |
JP5524094B2 (ja) | フュームド金属酸化物分散体の製造方法 | |
JP2011211178A (ja) | 研磨用組成物 | |
CA2469335A1 (fr) | Dispersions stables de nanoparticules dans un milieu aqueux | |
EP2106426A2 (fr) | Composition pour polir des surfaces de dioxyde de silicium | |
WO2018216218A1 (fr) | Dispersion dans un liquide contenant des nanobulles de particules fines d'un oxyde inorganique, abrasif la contenant, et procédés de production associés | |
KR19990023544A (ko) | 무기 입자의 수성 분산체와 그의 제조 방법 | |
JP6141482B1 (ja) | ナノバブル含有無機酸化物微粒子分散液、それを含む研磨剤およびそれらの製造方法 | |
KR20210116492A (ko) | 인산티타늄 분체, 화장료용 백색 안료 | |
JP4435391B2 (ja) | コロイド状シリカスラリー | |
WO2018221304A1 (fr) | Particules fines d'oxyde inorganique contenant des nanobulles, et agent de polissage comprenant celles-ci | |
DE102016122199A1 (de) | Halit-salze als siliziumcarbid-ätzmittel für eine erhöhung der cmp-materialabtragsrate bei sic-wafern | |
TWI715772B (zh) | 含有奈米氣泡之無機氧化物微粒子分散液、含有該分散液的研磨劑及此等之製造方法 | |
TW201532963A (zh) | 針狀碳酸鍶微粉末及其製造方法 | |
JP2001348214A (ja) | フラーレン水分散液の製造法 | |
WO2004063097A1 (fr) | Procede d'adjonction de charbon actif pour la purification de l'eau, et procede de purification de l'eau | |
Philipse | Preparation of boehmite—silica colloids: Rods, spheres, needles and gels | |
JP2015105217A (ja) | 粗大粒子添加によるナノ粒子スラリーの分散処理方法 | |
DE10239144A1 (de) | Dispersion | |
JP5215045B2 (ja) | フミン質及び/又はフミン質の誘導体の分散液の製造方法 | |
JP4716621B2 (ja) | 高濃度シリカスラリー及びシリカスラリーの製造方法 | |
JP6347134B2 (ja) | 炭酸ストロンチウム微粉末及びその製造方法 | |
JP2007008981A (ja) | フミン質分散液 | |
KR100885520B1 (ko) | 고체 미립자의 제조방법 및 이를 이용하여 제조된 고체미립자 | |
CN115491129A (zh) | 一种两性离子表面活性成分的化学机械抛光液 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 17911349 Country of ref document: EP Kind code of ref document: A1 |
|
NENP | Non-entry into the national phase |
Ref country code: DE |
|
122 | Ep: pct application non-entry in european phase |
Ref document number: 17911349 Country of ref document: EP Kind code of ref document: A1 |
|
NENP | Non-entry into the national phase |
Ref country code: JP |