WO2023013695A1 - Cmp用研磨液、cmp用研磨液セット及び研磨方法 - Google Patents
Cmp用研磨液、cmp用研磨液セット及び研磨方法 Download PDFInfo
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- WO2023013695A1 WO2023013695A1 PCT/JP2022/029843 JP2022029843W WO2023013695A1 WO 2023013695 A1 WO2023013695 A1 WO 2023013695A1 JP 2022029843 W JP2022029843 W JP 2022029843W WO 2023013695 A1 WO2023013695 A1 WO 2023013695A1
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- 229940090248 4-hydroxybenzoic acid Drugs 0.000 description 1
- CWJJAFQCTXFSTA-UHFFFAOYSA-N 4-methylphthalic acid Chemical compound CC1=CC=C(C(O)=O)C(C(O)=O)=C1 CWJJAFQCTXFSTA-UHFFFAOYSA-N 0.000 description 1
- WNKQDGLSQUASME-UHFFFAOYSA-N 4-sulfophthalic acid Chemical compound OC(=O)C1=CC=C(S(O)(=O)=O)C=C1C(O)=O WNKQDGLSQUASME-UHFFFAOYSA-N 0.000 description 1
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- 239000004475 Arginine Substances 0.000 description 1
- 238000004438 BET method Methods 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
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- 239000004471 Glycine Substances 0.000 description 1
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- 229930182816 L-glutamine Natural products 0.000 description 1
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- 238000002441 X-ray diffraction Methods 0.000 description 1
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- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000003927 aminopyridines Chemical class 0.000 description 1
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- 125000005577 anthracene group Chemical group 0.000 description 1
- ODKSFYDXXFIFQN-UHFFFAOYSA-N arginine Natural products OC(=O)C(N)CCCNC(N)=N ODKSFYDXXFIFQN-UHFFFAOYSA-N 0.000 description 1
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- 150000001558 benzoic acid derivatives Chemical class 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N beta-methyl-butyric acid Natural products CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
- 239000007998 bicine buffer Substances 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000005380 borophosphosilicate glass Substances 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 150000001767 cationic compounds Chemical class 0.000 description 1
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 description 1
- 229960001759 cerium oxalate Drugs 0.000 description 1
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 description 1
- 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 description 1
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 description 1
- XHKOOTFZHJHDTI-UHFFFAOYSA-K cerium(3+);tribromate Chemical compound [Ce+3].[O-]Br(=O)=O.[O-]Br(=O)=O.[O-]Br(=O)=O XHKOOTFZHJHDTI-UHFFFAOYSA-K 0.000 description 1
- GHLITDDQOMIBFS-UHFFFAOYSA-H cerium(3+);tricarbonate Chemical compound [Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O GHLITDDQOMIBFS-UHFFFAOYSA-H 0.000 description 1
- KHSBAWXKALEJFR-UHFFFAOYSA-H cerium(3+);tricarbonate;hydrate Chemical compound O.[Ce+3].[Ce+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O KHSBAWXKALEJFR-UHFFFAOYSA-H 0.000 description 1
- KKVSNHQGJGJMHA-UHFFFAOYSA-H cerium(3+);trisulfate;hydrate Chemical compound O.[Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O KKVSNHQGJGJMHA-UHFFFAOYSA-H 0.000 description 1
- MOOUSOJAOQPDEH-UHFFFAOYSA-K cerium(iii) bromide Chemical compound [Br-].[Br-].[Br-].[Ce+3] MOOUSOJAOQPDEH-UHFFFAOYSA-K 0.000 description 1
- UNJPQTDTZAKTFK-UHFFFAOYSA-K cerium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Ce+3] UNJPQTDTZAKTFK-UHFFFAOYSA-K 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 150000001923 cyclic compounds Chemical class 0.000 description 1
- 235000018417 cysteine Nutrition 0.000 description 1
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 description 1
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- 235000019800 disodium phosphate Nutrition 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 235000013922 glutamic acid Nutrition 0.000 description 1
- 239000004220 glutamic acid Substances 0.000 description 1
- ZDXPYRJPNDTMRX-UHFFFAOYSA-N glutamine Natural products OC(=O)C(N)CCC(N)=O ZDXPYRJPNDTMRX-UHFFFAOYSA-N 0.000 description 1
- 125000001072 heteroaryl group Chemical group 0.000 description 1
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- 125000000623 heterocyclic group Chemical group 0.000 description 1
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- 125000002883 imidazolyl group Chemical group 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229960004705 kojic acid Drugs 0.000 description 1
- 238000001459 lithography Methods 0.000 description 1
- 229940043353 maltol Drugs 0.000 description 1
- 229960002510 mandelic acid Drugs 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000005121 nitriding Methods 0.000 description 1
- JCXJVPUVTGWSNB-UHFFFAOYSA-N nitrogen dioxide Inorganic materials O=[N]=O JCXJVPUVTGWSNB-UHFFFAOYSA-N 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- WHSXTWFYRGOBGO-UHFFFAOYSA-N o-cresotic acid Natural products CC1=CC=CC(C(O)=O)=C1O WHSXTWFYRGOBGO-UHFFFAOYSA-N 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 238000001139 pH measurement Methods 0.000 description 1
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- IUGYQRQAERSCNH-UHFFFAOYSA-N pivalic acid Chemical compound CC(C)(C)C(O)=O IUGYQRQAERSCNH-UHFFFAOYSA-N 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 159000000001 potassium salts Chemical class 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000003217 pyrazoles Chemical class 0.000 description 1
- 125000002943 quinolinyl group Chemical group N1=C(C=CC2=CC=CC=C12)* 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- ORIHZIZPTZTNCU-YVMONPNESA-N salicylaldoxime Chemical compound O\N=C/C1=CC=CC=C1O ORIHZIZPTZTNCU-YVMONPNESA-N 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
- 238000000733 zeta-potential measurement Methods 0.000 description 1
Images
Classifications
-
- 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
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
-
- 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
-
- 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
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3105—After-treatment
- H01L21/31051—Planarisation of the insulating layers
- H01L21/31053—Planarisation of the insulating layers involving a dielectric removal step
Definitions
- the present disclosure relates to a polishing liquid for CMP (Chemical Mechanical Polishing), a polishing liquid set for CMP, a polishing method, and the like.
- CMP Chemical Mechanical Polishing
- CMP technology is one of the most important technologies in the process of manufacturing a device with multi-layered wiring.
- CMP technology is a technology for flattening the surface of a substrate obtained by forming a thin film on a substrate by chemical vapor deposition (CVD) or the like.
- CVD chemical vapor deposition
- planarization by CMP is essential to ensure the depth of focus of lithography. If the surface of the substrate has irregularities, problems such as the impossibility of focusing in the exposure process and the inability to sufficiently form a fine wiring structure occur.
- CMP technology forms element isolation (isolation between elements; STI: Shallow Trench Isolation) regions by polishing plasma oxide films (BPSG, HDP-SiO 2 , p-TEOS, etc.) in the device manufacturing process.
- step of forming an ILD film interlayer insulating film; an insulating film that electrically insulates metal members (such as wiring) in the same layer); , Al/Cu plugs).
- the CMP is usually performed using a device capable of supplying a polishing liquid onto the polishing pad. Then, the surface of the substrate is polished by pressing the substrate against the polishing pad while supplying a polishing liquid between the surface of the substrate and the polishing pad.
- the polishing liquid is one of the elemental technologies, and in order to obtain a high-performance polishing liquid, various polishing liquids have been developed (for example, Patent Document 1 below). reference).
- a silica-based polishing liquid (polishing liquid using abrasive grains containing silica-based particles) having a high polishing rate is mainly used (for example, see Patent Document 2 below).
- a silica-based polishing liquid it tends to be difficult to control polishing scratches that cause defects.
- JP 2008-288537 A JP-A-9-316431 JP-A-10-102038
- a silicon oxide blanket wafer having no uneven pattern has a fine uneven pattern composed of convex portions (eg, Line portions) and concave portions (eg, Space portions). It may be desired to obtain a high polishing rate ratio of silicon oxide on the protrusions of the patterned wafer.
- the pressure applied to the convex portions during polishing tends to be greater than the main surface of a blanket wafer having no concave and convex pattern.
- the polishing rate ratio at the convex portion of the wafer is high, the present inventor decided to increase the pH of the CMP polishing liquid using saturated monocarboxylic acid to 4.0 in order to improve the dispersibility of the abrasive grains. , a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer may not be obtained.
- the present disclosure relates to the following [1] to [22] and the like.
- Abrasive grains, an additive, and water wherein the abrasive grains contain cerium-based particles, and the additive is (A1) a 4-pyrone-based compound represented by the following general formula (1)
- a polishing liquid for CMP containing a compound and (B) a saturated monocarboxylic acid, and having a pH exceeding 4.0.
- X 11 , X 12 and X 13 are each independently a hydrogen atom or a monovalent substituent.
- Component (A1) is 3-hydroxy-2-methyl-4-pyrone, 5-hydroxy-2-(hydroxymethyl)-4-pyrone, and 2-ethyl-3-hydroxy-4-pyrone
- the polishing liquid for CMP according to any one of [1] to [10], which has a pH of 8.0 or less.
- a polishing liquid for CMP comprising: a pH greater than 4.0.
- [15] The polishing liquid for CMP according to any one of [12] to [14], wherein the content of component (B) is 0.0001 to 5% by mass.
- the constituent components of the polishing liquid for CMP according to any one of [1] to [19] are stored separately as a first liquid and a second liquid, and the first liquid is the A polishing liquid set for CMP, containing abrasive grains and water, wherein the second liquid contains at least one of the additives and water.
- the polishing liquid for CMP according to any one of [1] to [19], or the first liquid and the second liquid in the polishing liquid set for CMP according to [20] A polishing method comprising a step of polishing a surface to be polished using a CMP polishing liquid obtained by mixing.
- the polishing method according to [21], wherein the surface to be polished contains silicon oxide.
- a CMP polishing liquid capable of achieving a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer.
- a CMP polishing liquid set for obtaining the CMP polishing liquid.
- FIG. 4 is a schematic cross-sectional view showing the process of polishing an ILD film
- a numerical range indicated using “-” indicates a range that includes the numerical values before and after "-" as the minimum and maximum values, respectively.
- “A or more” in a numerical range means A and a range exceeding A.
- “A or less” in a numerical range means A and a range less than A.
- the upper limit value or lower limit value of the numerical range in one step can be arbitrarily combined with the upper limit value or lower limit of the numerical range in another step.
- the upper or lower limits of the numerical ranges may be replaced with the values shown in the examples.
- “A or B” may include either A or B, or may include both.
- each component in the composition means the total amount of the plurality of substances present in the composition unless otherwise specified when there are multiple substances corresponding to each component in the composition.
- layer or film includes not only a shape structure formed over the entire surface but also a shape structure formed partially when viewed as a plan view.
- process is included in the term not only as an independent process, but also as long as the intended action of the process is achieved even if it is not clearly distinguishable from other processes.
- the CMP polishing liquid according to the present embodiment contains abrasive grains, an additive, and water. (referred to as "polishing liquid”).
- the abrasive grains contain cerium-based particles (particles containing a cerium-based compound).
- the additives of the polishing liquid according to the first embodiment are (A1) a 4-pyrone compound represented by the following general formula (1) (component (A1)) and (B) a saturated monocarboxylic acid ((B) components) and
- the additive of the polishing liquid according to the second embodiment includes (A2) picolinic acid (component (A2)) and (B) saturated monocarboxylic acid (component (B)).
- the additive of the polishing liquid according to the present embodiment may contain component (A1), component (A2) and component (B).
- the pH of the CMP polishing liquid according to this embodiment exceeds 4.0.
- X 11 , X 12 and X 13 are each independently a hydrogen atom or a monovalent substituent. ]
- a silicon oxide blanket wafer having no uneven pattern has a fine uneven pattern composed of convex portions (eg, Line portions) and concave portions (eg, Space portions). It is possible to achieve a high polishing rate ratio of silicon oxide on the convex portions of the patterned wafer. It is possible to achieve a high polishing rate ratio for the silicon oxide of the protrusions in the region of 80 ⁇ m.
- the factors that enable a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer to be achieved are not necessarily clear, but are presumed to be as follows. However, the factors are not limited to the following contents. That is, according to the polishing liquid according to the present embodiment, when the pH of the polishing liquid for CMP using the component (B) (saturated monocarboxylic acid) exceeds 4.0, the component (A1) or the component (A2) is By using it, the interaction between the polishing liquid and the silicon oxide of the protrusions increases (for example, the chemical reaction between the cerium-based particles in the polishing liquid and the silicon oxide of the protrusions (derived from the bonding of Si—O—Ce reaction) is promoted).
- high-speed polishing of silicon oxide for example, a polishing rate of 100 nm/min or more (preferably 250 nm/min or more), etc.) on a blanket wafer having no uneven pattern is achieved.
- a polishing rate of silicon oxide for example, a polishing rate of 100 nm/min or more (preferably 250 nm/min or more), etc.
- the polishing liquid according to the present embodiment it is possible to obtain a sufficiently low polishing rate for silicon nitride and obtain high polishing selectivity of silicon oxide to silicon nitride. In this case, it is suitable for polishing when forming an element isolation region.
- the polishing rate of silicon nitride on a blanket wafer is, for example, less than 2.0 nm/min (preferably less than 1.0 nm/min etc.) can be obtained.
- the polishing liquid according to this embodiment can be used for CMP of semiconductor wafer materials, and can be used, for example, for polishing a silicon oxide film provided on the surface of a semiconductor wafer.
- the polishing liquid according to this embodiment can be used in the CMP process of the ILD film. According to one aspect of the polishing liquid according to the present embodiment, it is possible to obtain a high polishing rate, suppress the aggregation of abrasive grains and the occurrence of polishing scratches, and obtain high flatness.
- the abrasive grains contain cerium-based particles. By using the cerium-based particles as the abrasive grains, it is easy to obtain a high polishing rate of silicon oxide on the convex portions of the pattern wafer while reducing polishing scratches on the surface to be polished.
- Cerium-based compounds of cerium-based particles include cerium oxide, cerium hydroxide, cerium ammonium nitrate, cerium acetate, cerium sulfate hydrate, cerium bromate, cerium bromide, cerium chloride, cerium oxalate, cerium nitrate, cerium carbonate, etc. are mentioned.
- cerium-based particles containing cerium oxide (cerium oxide particles)
- the cerium oxide particles may contain polycrystalline cerium oxide having grain boundaries. Such polycrystalline cerium oxide particles have the property that active surfaces appear one after another as they become finer during polishing, and can maintain a high polishing rate of silicon oxide on convex portions of a pattern wafer.
- Examples of methods for producing cerium oxide particles include a calcination method and an oxidation method using hydrogen peroxide.
- the firing temperature may be 350 to 900°C. If the cerium oxide particles produced are agglomerated, the particles may be mechanically crushed.
- the pulverization method may be, for example, dry pulverization using a jet mill or the like, or wet pulverization using a planetary bead mill or the like.
- the jet mill for example, the one described in "Kagaku Kogaku Ronbunshu", Vol. 6, No. 5, (1980), pp. 527-532 can be used.
- the zeta-potential (surface potential) of the abrasive grains in the polishing liquid is considered to facilitate high-speed polishing of silicon oxide on the convex portions of patterned wafers, and high-speed polishing of silicon oxide on blanket wafers without uneven patterns. From the standpoint of ease of attainment, it may be positive (zeta potential may exceed 0 mV).
- the zeta potential of abrasive grains can be measured using, for example, a dynamic light scattering zeta potential measuring device (eg, trade name: DelsaNano C manufactured by Beckman Coulter, Inc.).
- the zeta potential of abrasive grains can be adjusted using additives. For example, abrasive grains having a positive zeta potential can be obtained by contacting the abrasive grains with an acid component (eg, acetic acid).
- the average particle size of the abrasive grains is 50 nm from the viewpoint of easily obtaining a high polishing rate of silicon oxide on the convex portions of the pattern wafer and from the viewpoint of easily achieving high-speed polishing of silicon oxide on a blanket wafer having no uneven pattern. 70 nm or more, 100 nm or more, more than 100 nm, 105 nm or more, 110 nm or more, 115 nm or more, 120 nm or more, 125 nm or more, 130 nm or more, 135 nm or more, or 140 nm or more.
- the average grain size of the abrasive grains is 500 nm or less, 300 nm or less, 200 nm or less, 180 nm or less, 150 nm or less, 140 nm or less, 135 nm or less, 130 nm or less, 125 nm or less, or 120 nm or less.
- the average grain size of the abrasive grains is 50 to 500 nm, 50 to 200 nm, 50 to 150 nm, 70 to 500 nm, 70 to 200 nm, 70 to 150 nm, 100 to 500 nm, 100 to 200 nm, or 100 to 150 nm.
- the average grain size of the abrasive grains it is possible to efficiently obtain a high-speed polishing rate and low scratch properties for silicon oxide in accordance with the average grain size of the abrasive grains.
- Average particle diameter of abrasive grains means the median value of the volume distribution of a sample of slurry in which abrasive grains are dispersed, measured with a laser diffraction/scattering particle size distribution measuring device, MicrotracBEL Corp. product name: Microtrac MT3300EXII or the like.
- a sample is prepared by adjusting the content of abrasive grains by dispersing abrasive grains in water so that the content of abrasive grains is 0.25% by mass based on the total mass of the sample, and this sample is measured. Set in the device and measure the median volume distribution.
- the content of abrasive grains may be within the following ranges based on the total mass of the polishing liquid, from the viewpoint of achieving an excellent balance between the polishing rate of silicon oxide on the convex portions of the pattern wafer and the dispersion stability of the abrasive grains.
- the content of abrasive grains is 0.01% by mass or more, 0.05% by mass or more, 0.1% by mass or more, 0.15% by mass or more, 0.2% by mass or more, 0.25% by mass or more, 0 .3% by mass or more, 0.5% by mass or more, 0.8% by mass or more, or 1% by mass or more.
- the content of abrasive grains is 10% by mass or less, 5% by mass or less, 3% by mass or less, 1% by mass or less, 0.8% by mass or less, 0.5% by mass or less, 0.3% by mass or less, or It may be 0.25% by mass or less.
- the content of abrasive grains is 0.01 to 10% by mass, 0.01 to 1% by mass, 0.01 to 0.5% by mass, 0.01 to 0.25% by mass, 0.01% to 0.25% by mass, 05 to 10% by mass, 0.05 to 1% by mass, 0.05 to 0.5% by mass, 0.05 to 0.25% by mass, 0.1 to 10% by mass, 0.1 to 1% by mass, It may be 0.1 to 0.5 mass %, or 0.1 to 0.25 mass %.
- the additive of the polishing liquid according to the first embodiment includes, as the (A1) component, a 4-pyrone compound represented by the general formula (1) (hereinafter sometimes simply referred to as "4-pyrone compound").
- a 4-pyrone compound represented by the general formula (1)
- the 4-pyrone compound is an additive that can increase the interaction between the polishing liquid and silicon oxide, it does not have the effect of weakening the repulsive force such as the electrostatic repulsive force between abrasive grains. , it is thought that the agglomeration of abrasive grains can be suppressed.
- a 4-pyrone-based compound is a compound represented by the following general formula (1), and is a compound having a structure in which a hydroxy group is bonded to a carbon atom adjacent to a carbon atom of a carbonyl group.
- a "4-pyrone compound” is a heterocyclic compound having an oxy group and a carbonyl group, and a ⁇ -pyrone ring (6-membered ring) in which the carbonyl group is located at the 4-position relative to the oxy group. .
- a hydroxy group is bonded to the carbon atom adjacent to the carboxy group in the ⁇ -pyrone ring, and the other carbon atoms are substituted with substituents other than hydrogen atoms. good too.
- X 11 , X 12 and X 13 each independently represent a hydrogen atom or a monovalent substituent.
- monovalent substituents include aldehyde group, hydroxy group, carboxyl group, carboxylic acid group, sulfonic acid group, phosphoric acid group, bromine atom, chlorine atom, iodine atom, fluorine atom, nitro group, hydrazine group, alkyl group ( Examples thereof include an alkyl group having 1 to 8 carbon atoms), an aryl group (eg an aryl group having 6 to 12 carbon atoms), an alkenyl group (eg an alkenyl group having 1 to 8 carbon atoms).
- Alkyl groups, aryl groups and alkenyl groups may be substituted with OH, COOH, Br, Cl, I, NO2 and the like.
- the substituents may be attached to the carbon atoms adjacent to the oxy group, i.e. X 11 and X 12 may be substituents .
- At least two of X 11 , X 12 and X 13 may be hydrogen atoms.
- the 4-pyrone-based compound has a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer, and from the viewpoint of easily suppressing the aggregation of abrasive grains, 3-hydroxy -2-methyl-4-pyrone (alias: 3-hydroxy-2-methyl-4H-pyran-4-one, maltol), 5-hydroxy-2-(hydroxymethyl)-4-pyrone (alias: 5-hydroxy -2-(hydroxymethyl)-4H-pyran-4-one, kojic acid) and 2-ethyl-3-hydroxy-4-pyrone (alias: 2-ethyl-3-hydroxy-4H-pyran-4- on), and may include 3-hydroxy-2-methyl-4-pyrone.
- the 4-pyrone compounds can be used singly or in combination of two or more.
- the 4-pyrone compound may be water-soluble.
- a compound with high solubility in water By using a compound with high solubility in water, the desired amount of additive can be dissolved in the polishing liquid, and the effect of improving the polishing speed and suppressing the aggregation of abrasive grains can be improved to a higher level. can be achieved.
- the solubility of the 4-pyrone compound in 100 g of water at room temperature (25° C.) may be 0.001 g or more, 0.005 g or more, 0.01 g or more, or 0.05 g or more.
- the upper limit of solubility is not particularly limited.
- the content of the 4-pyrone-based compound is within the following range based on the total mass of the polishing liquid, from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer. It can be.
- the content of the 4-pyrone compound is 0.001 mass% or more, 0.005 mass% or more, 0.01 mass% or more, 0.015 mass% or more, 0.02 mass% or more, 0.025 mass% 0.03% by mass or more, 0.032% by mass or more, 0.034% by mass or more, 0.035% by mass or more, 0.04% by mass or more, 0.05% by mass or more, 0.08% by mass or more , 0.1% by mass or more, 0.13% by mass or more, 0.15% by mass or more, 0.18% by mass or more, or 0.2% by mass or more.
- the content of the 4-pyrone compound is 5% by mass or less, 3% by mass or less, 1% by mass or less, 0.8% by mass or less, 0.5% by mass or less, 0.3% by mass or less, and 0.2% by mass. % or less, 0.18 mass % or less, 0.15 mass % or less, 0.13 mass % or less, 0.1 mass % or less, 0.08 mass % or less, 0.05 mass % or less, 0.04 mass % Below, it may be 0.035% by mass or less, or 0.034% by mass or less. From these viewpoints, the content of the 4-pyrone compound is 0.001 to 5% by mass, 0.001 to 1% by mass, 0.001 to 0.3% by mass, and 0.001 to 0.1% by mass.
- 0.001 to 0.05% by mass 0.01 to 5% by mass, 0.01 to 1% by mass, 0.01 to 0.3% by mass, 0.01 to 0.1% by mass, 0.01 ⁇ 0.05% by mass, 0.02-5% by mass, 0.02-1% by mass, 0.02-0.3% by mass, 0.02-0.1% by mass, or 0.02-0 0.05% by weight.
- the mass ratio A of the content of the 4-pyrone-based compound to the content of the abrasive grains (4-pyrone-based compound/abrasive grains) is a high polishing rate of silicon oxide on the convex portions of the pattern wafer with respect to silicon oxide on the blanket wafer. From the viewpoint of easily obtaining the ratio, the following ranges may be used.
- the mass ratio A is 0.01 or more, 0.03 or more, 0.5 or more, 0.08 or more, 0.1 or more, 0.12 or more, 0.13 or more, 0.15 or more, 0.18 or more, Alternatively, it may be 0.2 or more.
- Mass ratio A is 1 or less, less than 1, 0.8 or less, 0.6 or less, 0.5 or less, 0.4 or less, 0.3 or less, 0.2 or less, 0.18 or less, 0.15 or less , 0.13 or less, 0.12 or less, or 0.1 or less. From these viewpoints, the mass ratio A is 0.01 to 1, 0.01 to 0.3, 0.01 to 0.15, 0.1 to 1, 0.1 to 0.3, 0.1 to It may be 0.15, 0.12-1, 0.12-0.3, or 0.12-0.15.
- the additive of the polishing liquid according to the second embodiment contains picolinic acid as the (A2) component. It is presumed that the use of the component (A2) increases the interaction between the polishing liquid and the silicon oxide, thereby increasing the polishing rate.
- the content of picolinic acid may be in the following range based on the total mass of the polishing liquid, from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer. .
- the content of picolinic acid is 0.001% by mass or more, 0.005% by mass or more, 0.01% by mass or more, 0.03% by mass or more, 0.05% by mass or more, 0.08% by mass or more, 0 0.1% by mass or more, 0.12% by mass or more, 0.15% by mass or more, 0.18% by mass or more, or 0.2% by mass or more.
- the content of picolinic acid is 5% by mass or less, 3% by mass or less, 1% by mass or less, 0.8% by mass or less, 0.5% by mass or less, 0.4% by mass or less, 0.3% by mass or less, Alternatively, it may be 0.2% by mass or less. From these viewpoints, the content of picolinic acid is 0.001 to 5% by mass, 0.001 to 1% by mass, 0.001 to 0.5% by mass, 0.001 to 0.3% by mass, 01 to 5% by mass, 0.01 to 1% by mass, 0.01 to 0.5% by mass, 0.01 to 0.3% by mass, 0.1 to 5% by mass, 0.1 to 1% by mass, It may be from 0.1 to 0.5 mass %, or from 0.1 to 0.3 mass %.
- the mass ratio A2 of the content of picolinic acid to the content of abrasive grains is from the viewpoint that a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer can be easily obtained. to the following range.
- Mass ratio A2 is 0.01 or more, 0.03 or more, 0.05 or more, 0.08 or more, 0.1 or more, 0.12 or more, 0.15 or more, 0.18 or more, or 0.2 or more.
- the mass ratio A2 is 1 or less, less than 1, 0.8 or less, 0.6 or less, 0.5 or less, 0.4 or less, 0.3 or less, 0.25 or less, or 0.2 or less good.
- the mass ratio A2 is 0.01 to 1, 0.01 to 0.5, 0.01 to 0.3, 0.01 to 0.2, 0.05 to 1, 0.05 to 0.5, 0.05-0.3, 0.05-0.2, 0.1-1, 0.1-0.5, 0.1-0.3, or 0.1-0. can be two.
- the additive of the polishing liquid according to this embodiment contains a saturated monocarboxylic acid as the component (B).
- the component (B) can be used for the purpose of improving the dispersibility of abrasive grains.
- the component (B) can also contribute to the adjustment of the polishing rate ratio of silicon oxide on the projections of the pattern wafer to the silicon oxide on the blanket wafer, the polishing rate of silicon nitride that can be used as a stopper material, and the like.
- Saturated monocarboxylic acids include acetic acid, propionic acid, butyric acid, isobutyric acid, valeric acid, isovaleric acid, pivalic acid, hydroangelic acid, caproic acid, 2-methylpentanoic acid, 4-methylpentanoic acid, 2,3- dimethylbutanoic acid, 2-ethylbutanoic acid, 2,2-dimethylbutanoic acid, 3,3-dimethylbutanoic acid and the like.
- the number of carbon atoms in the saturated monocarboxylic acid is 1 to 6, 2 to 6, 1 to 4, and 2 from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer.
- Saturated monocarboxylic acid has the viewpoint that it is easy to obtain a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to the silicon oxide on the blanket wafer, and the viewpoint that the effect of suppressing the polishing rate of silicon nitride can be effectively obtained.
- the content of the saturated monocarboxylic acid makes it easy to obtain a high polishing rate ratio of the silicon oxide on the convex portions of the pattern wafer to the silicon oxide on the blanket wafer, and effectively obtains the effect of suppressing the polishing rate of silicon nitride. from the standpoint of being able to handle the total mass of the polishing liquid as a reference, it may be in the following ranges.
- the content of saturated monocarboxylic acid is 0.0001% by mass or more, 0.0003% by mass or more, 0.0005% by mass or more, 0.001% by mass or more, 0.002% by mass or more, 0.005% by mass or more , 0.01% by mass or more, 0.02% by mass or more, 0.03% by mass or more, 0.04% by mass or more, 0.045% by mass or more, 0.05% by mass or more, 0.1% by mass or more, It may be 0.2% by mass or more, 0.3% by mass or more, or 0.4% by mass or more.
- the content of saturated monocarboxylic acid is 5% by mass or less, 3% by mass or less, 1% by mass or less, 0.5% by mass or less, 0.4% by mass or less, 0.3% by mass or less, and 0.2% by mass. 0.1% by mass or less, 0.05% by mass or less, 0.045% by mass or less, 0.04% by mass or less, 0.03% by mass or less, 0.02% by mass or less, 0.01% by mass or less , or 0.005% by mass or less.
- the content of the saturated monocarboxylic acid is 0.0001 to 5% by mass, 0.0001 to 1% by mass, 0.0001 to 0.1% by mass, 0.0001 to 0.05% by mass, 0.01 to 5% by mass, 0.01 to 1% by mass, 0.01 to 0.1% by mass, 0.01 to 0.05% by mass, 0.03 to 5% by mass, 0.03 to 1% by mass %, 0.03-0.1% by weight, or 0.03-0.05% by weight.
- the mass ratio B1 of the content of saturated monocarboxylic acid to the content of abrasive grains provides a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer. From the standpoint of ease of obtaining, the following ranges may be used.
- the mass ratio B1 is 0.001 or more, 0.002 or more, 0.005 or more, 0.01 or more, 0.05 or more, 0.1 or more, 0.15 or more, 0.2 or more, 0.5 or more, It may be 1 or more, more than 1, or 1.5 or more.
- the mass ratio B1 is 10 or less, 5 or less, 2 or less, 1.5 or less, 1 or less, less than 1, 0.5 or less, 0.2 or less, 0.15 or less, 0.1 or less, 0.05 or less, It may be 0.01 or less, 0.005 or less, or 0.002 or less. From these viewpoints, the mass ratio B1 is 0.001 to 10, 0.001 to 2, 0.001 to 0.5, 0.05 to 10, 0.05 to 2, 0.05 to 0.5, It may be 0.1-10, 0.1-2, or 0.1-0.5.
- the mass ratio B2 of the content of saturated monocarboxylic acid to the content of component (A1) is From the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer, the range may be as follows. Mass ratio B2 is 0.001 or more, 0.005 or more, 0.01 or more, 0.02 or more, 0.05 or more, 0.1 or more, 0.5 or more, 0.8 or more, 1 or more, 1. It may be 5 or more, 2 or more, 5 or more, or 10 or more.
- the mass ratio B2 is 20 or less, 10 or less, 5 or less, 2 or less, 1.5 or less, 1 or less, 0.8 or less, 0.5 or less, 0.1 or less, 0.05 or less, 0.02 or less, It may be 0.015 or less, or 0.1 or less. From these viewpoints, the mass ratio B2 is 0.001 to 20, 0.001 to 5, 0.001 to 2, 0.05 to 20, 0.05 to 5, 0.05 to 2, 1 to 20, It may be 1-5, or 1-2.
- the mass ratio B3 of the content of saturated monocarboxylic acid to the content of component (A2) (saturated monocarboxylic acid/component (A2)) is From the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer, the range may be as follows.
- the mass ratio B3 may be 0.001 or more, 0.003 or more, 0.005 or more, 0.008 or more, or 0.01 or more.
- the mass ratio B3 is 1 or less, less than 1, 0.5 or less, 0.1 or less, 0.08 or less, 0.05 or less, 0.03 or less, 0.02 or less, or 0.01 or less good.
- the mass ratio B3 is 0.001 to 1, 0.001 to 0.5, 0.001 to 0.1, 0.005 to 1, 0.005 to 0.5, 0.005 to It may be 0.1, 0.01-1, 0.01-0.5, or 0.01-0.1.
- the additive of the polishing liquid according to the present embodiment includes, as the component (C), a compound having two or more nitrogen atoms to which a hydroxyalkyl group is bonded (nitrogen-containing hydroxyalkyl compound; however, a compound corresponding to the component (A1) ) may be included.
- the component (C) the interaction between the polishing solution and the silicon oxide of the convex portions in the concave-convex pattern is increased, so that a high polishing rate of the silicon oxide of the convex portions can be easily obtained, and at the same time, nitriding that can be used as a stopper material It is easy to suppress the polishing rate of silicon.
- component (C) the hydroxyalkyl group is directly bonded to the nitrogen atom, and the hydroxy group is directly bonded to the alkyl group directly bonded to the nitrogen atom.
- Component (C) can use an alkyl group having no substituent other than a hydroxy group as the hydroxyalkyl group bonded to the nitrogen atom.
- Component (C) is composed of two hydroxy It may include compounds having a nitrogen atom attached to an alkyl group, and may include compounds having two or more nitrogen atoms attached to two hydroxyalkyl groups.
- the number of nitrogen atoms in one molecule in the component (C) is such that a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer is easily obtained, and the polishing rate of silicon nitride is increased. It may be 2 to 5, 2 to 4, or 2 to 3 from the viewpoint of easy suppression.
- the number of hydroxy groups in one molecule in the component (C) is such that a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer is easily obtained, and the polishing rate of silicon nitride is increased. From the viewpoint of easy suppression, it may be 2 to 6, 2 to 5, 2 to 4, 3 to 6, 3 to 5, 3 to 4, 4 to 6, or 4 to 5.
- Component (C) is a nitrogen atom from the viewpoint that a high polishing rate ratio of silicon oxide on the convex portion of the pattern wafer to the silicon oxide on the blanket wafer can be easily obtained, and from the viewpoint of easily suppressing the polishing rate of silicon nitride.
- a hydroxyalkyl group having 1 to 4 carbon atoms, 2 to 4 carbon atoms, 3 to 4 carbon atoms, 1 to 3 carbon atoms, 2 to 3 carbon atoms, or 1 to 2 carbon atoms may be used as the bonding hydroxyalkyl group.
- Component (C) is a nitrogen atom from the viewpoint that a high polishing rate ratio of silicon oxide on the convex portion of the pattern wafer to the silicon oxide on the blanket wafer can be easily obtained, and from the viewpoint of easily suppressing the polishing rate of silicon nitride.
- a hydroxyalkyl group having 1 to 3 or 1 to 2 hydroxy groups may be used as the bonding hydroxyalkyl group.
- Component (C) is a hydroxyalkyl group from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to the silicon oxide on the blanket wafer, and from the viewpoint of easily suppressing the polishing rate of silicon nitride.
- the component (C) has the following general formula from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to the silicon oxide on the blanket wafer, and from the viewpoint of easily suppressing the polishing rate of silicon nitride. It may contain a compound represented by (I).
- n is an integer of 1 or more
- R 11 , R 12 , R 13 and R 14 each independently represent a hydrogen atom or an organic group, and one or both of R 11 and R 12 are hydroxy an alkyl group and one or both of R 13 and R 14 is a hydroxyalkyl group.
- n may be in the range described above as the number of carbon atoms in the alkylene group between the two nitrogen atoms to which the hydroxyalkyl group is attached.
- the organic group may be a substituted or unsubstituted alkyl group, a hydroxyalkyl group, or a group having a nitrogen atom to which a hydroxyalkyl group is attached.
- Substituents for the alkyl group include a hydroxy group, a carboxy group, an amino group, a sulfo group, a nitro group and the like.
- R 11 , R 12 , R 13 or R 14 is a hydroxyalkyl group
- the number of carbon atoms in the hydroxyalkyl group may be within the range described above as the number of carbon atoms in the hydroxyalkyl group bonded to the nitrogen atom.
- ethylenedinitrilotetraethanol TBEED: 2,2′,2′′,2′′′-ethylenedinitrilotetraethanol (alias: N,N,N′,N′-Tetrakis (2 -hydroxyethyl) ethylenediamine), etc.
- ethylenedinitrilotetrapropanol EDTP: 1,1',1'',1'''-ethylenedinitrilotetra-2-propanol (alias: N,N,N',N' -Tetrakis(2-hydroxypropyl)ethylenediamine), N,N,N',N'',N'-pentakis(2-hydroxypropyl)diethylenetriamine, and the like.
- Component (C) is ethylene dinitrilo from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to the silicon oxide on the blanket wafer, and from the viewpoint of easily suppressing the polishing rate of silicon nitride. It may contain at least one selected from the group consisting of tetraethanol and ethylenedinitrilotetrapropanol, may contain ethylenedinitrilotetraethanol, and may contain ethylenedinitrilotetrapropanol.
- the component (C) contains a carboxy group from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to the silicon oxide on the blanket wafer, and from the viewpoint of easily suppressing the polishing rate of silicon nitride.
- the molecular weight of the component (C) is selected from the viewpoints of easily obtaining a high polishing rate ratio of the silicon oxide on the convex portions of the pattern wafer to the silicon oxide on the blanket wafer, and from the viewpoint of easily suppressing the polishing rate of the silicon nitride.
- Component (C) may be in the range of Component (C) has a molecular weight of 50 or more, 60 or more, 70 or more, 80 or more, 85 or more, 90 or more, 100 or more, 110 or more, 120 or more, 123 or more, 125 or more, 130 or more, 140 or more, 148 or more, It may be 150 or more, 160 or more, 170 or more, 180 or more, 200 or more, 210 or more, 230 or more, 250 or more, more than 250, or 280 or more.
- the molecular weight of component (C) is 1000 or less, less than 1000, 900 or less, 800 or less, 700 or less, 600 or less, 500 or less, 400 or less, 350 or less, 300 or less, 280 or less, 250 or less, less than 250, or 240. may be: From these viewpoints, the molecular weight of component (C) is 50 to 1000, 50 to 500, 50 to 300, 50 to 250, 200 to 1000, 200 to 500, 200 to 300, 200 to 250, 250 to 1000, 250 ⁇ 500, or 250-300.
- the content of the component (C) is the content of ethylenedinitrilotetraethanol, or the content of ethylenedinitrilotetrapropanol
- the content C1 is
- the following ranges may be used based on the total mass of the polishing liquid. .
- Content C1 is 0.001% by mass or more, 0.005% by mass or more, 0.01% by mass or more, 0.015% by mass or more, 0.02% by mass or more, 0.025% by mass or more, 0.03 % by mass or more, 0.035% by mass or more, 0.04% by mass or more, 0.045% by mass or more, 0.05% by mass or more, 0.06% by mass or more, 0.08% by mass or more, 0.1% by mass % or more, or 0.11 mass % or more.
- the content C1 is 5% by mass or less, 3% by mass or less, 1% by mass or less, 0.5% by mass or less, 0.4% by mass or less, 0.3% by mass or less, 0.2% by mass or less, 0.2% by mass or less.
- the content C1 is 0.001 to 5% by mass, 0.001 to 1% by mass, 0.001 to 0.1% by mass, 0.001 to 0.05% by mass, 0.01 to 5% by mass, 0.01 to 1% by mass, 0.01 to 0.1% by mass, 0.01 to 0.05% by mass, 0.02 to 5% by mass, 0.02 to 1% by mass, 0. 02 to 0.1 mass %, or 0.02 to 0.05 mass %.
- the content of component (C) the content of ethylenedinitrilotetraethanol, or the content of ethylenedinitrilotetrapropanol
- the content C2 is
- the following ranges may be used based on the total mass of the polishing liquid. .
- Content C2 is 0.001% by mass or more, 0.005% by mass or more, 0.01% by mass or more, 0.015% by mass or more, 0.02% by mass or more, 0.025% by mass or more, 0.03 % by mass or more, 0.035% by mass or more, 0.04% by mass or more, 0.045% by mass or more, 0.05% by mass or more, 0.06% by mass or more, 0.08% by mass or more, 0.1% by mass % or more, 0.12 mass % or more, 0.13 mass % or more, 0.15 mass % or more, 0.2 mass % or more, or 0.22 mass % or more.
- the content C2 is 5% by mass or less, 3% by mass or less, 1% by mass or less, 0.5% by mass or less, 0.4% by mass or less, 0.3% by mass or less, 0.22% by mass or less, 0.2% by mass or less.
- 2% by mass or less 0.15% by mass or less, 0.13% by mass or less, 0.12% by mass or less, 0.1% by mass or less, 0.08% by mass or less, 0.06% by mass or less, 0.05 % by mass or less, 0.045% by mass or less, 0.04% by mass or less, 0.035% by mass or less, 0.03% by mass or less, 0.025% by mass or less, or 0.02% by mass or less good.
- the content C2 is 0.001 to 5% by mass, 0.001 to 1% by mass, 0.001 to 0.3% by mass, 0.001 to 0.05% by mass, 0.01 to 5% by mass, 0.01 to 1% by mass, 0.01 to 0.3% by mass, 0.01 to 0.05% by mass, 0.02 to 5% by mass, 0.02 to 1% by mass, 0. 02 to 0.3 mass %, or 0.02 to 0.05 mass %.
- the mass ratio of the content of component (C) to the content of abrasive grains (component (C)/abrasive grains), the content of ethylenedinitrilotetraethanol to the content of abrasive grains (ethylenedinitrilotetraethanol/abrasive grains), or the mass ratio of the content of ethylenedinitrilotetrapropanol to the content of abrasive grains (ethylenedinitrilotetrapropanol/abrasive grains), the mass ratio C11 is From the viewpoint of easily obtaining a high polishing rate ratio of the silicon oxide on the convex portions of the pattern wafer to the silicon oxide on the blanket wafer, and from the viewpoint of easily suppressing the polishing rate of silicon nitride, the following ranges may be used.
- the mass ratio C11 is 0.001 or more, 0.005 or more, 0.01 or more, 0.02 or more, 0.03 or more, 0.05 or more, 0.08 or more, 0.1 or more, 0.12 or more, It may be 0.15 or more, 0.18 or more, or 0.2 or more.
- the mass ratio C11 is 10 or less, 5 or less, 2 or less, 1 or less, less than 1, 0.5 or less, 0.3 or less, 0.2 or less, 0.18 or less, 0.15 or less, 0.12 or less, It may be 0.1 or less, 0.08 or less, 0.05 or less, 0.03 or less, or 0.02 or less.
- the mass ratio C11 is 0.001 to 10, 0.001 to 1, 0.001 to 0.3, 0.001 to 0.1, 0.01 to 10, 0.01 to 1, It may be 0.01-0.3, 0.01-0.1, 0.02-10, 0.02-1, 0.02-0.3, or 0.02-0.1.
- the mass ratio of the content of component (C) to the content of abrasive grains (component (C)/abrasive grains), the content of ethylenedinitrilotetraethanol to the content of abrasive grains (ethylenedinitrilotetraethanol/abrasive grains), or the mass ratio of the content of ethylenedinitrilotetrapropanol to the content of abrasive grains (ethylenedinitrilotetrapropanol/abrasive grains), the mass ratio C21 is From the viewpoint of easily obtaining a high polishing rate ratio of the silicon oxide on the convex portions of the pattern wafer to the silicon oxide on the blanket wafer, and from the viewpoint of easily suppressing the polishing rate of silicon nitride, the following ranges may be used.
- the mass ratio C21 is 0.001 or more, 0.005 or more, 0.01 or more, 0.02 or more, 0.03 or more, 0.04 or more, 0.05 or more, 0.06 or more, 0.08 or more, It may be 0.1 or more, 0.13 or more, 0.15 or more, 0.2 or more, or 0.22 or more.
- the mass ratio C21 is 10 or less, 5 or less, 2 or less, 1 or less, less than 1, 0.5 or less, 0.3 or less, 0.25 or less, 0.22 or less, 0.2 or less, 0.15 or less, It may be 0.13 or less, 0.1 or less, 0.08 or less, 0.06 or less, 0.05 or less, 0.04 or less, 0.03 or less, or 0.02 or less.
- the mass ratio C21 is 0.001 to 10, 0.001 to 1, 0.001 to 0.3, 0.001 to 0.2, 0.01 to 10, 0.01 to 1, It may be 0.01-0.3, 0.01-0.2, 0.03-10, 0.03-1, 0.03-0.3, or 0.03-0.2.
- the mass ratio of the content of component (C) to the content of component (A1) ((C) component/(A1) component),
- the mass ratio C12 is from the viewpoint that a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer is easily obtained, and the polishing rate of silicon nitride is easily suppressed.
- the mass ratio C12 is 0.01 or more, 0.05 or more, 0.1 or more, 0.15 or more, 0.2 or more, 0.3 or more, 0.5 or more, 0.6 or more, 0.8 or more, It may be 0.85 or greater, 0.9 or greater, 1 or greater, greater than 1, 1.1 or greater, 1.2 or greater, 1.4 or greater, or 1.5 or greater.
- the mass ratio C12 is 10 or less, 8 or less, 5 or less, 2 or less, 1.5 or less, 1.4 or less, 1.2 or less, 1.1 or less, 1 or less, less than 1, 0.9 or less, 0.9 or less.
- the mass ratio C12 is 0.01-10, 0.01-2, 0.01-1, 0.01-0.5, 0.05-10, 0.05-2, 0.01-10. 05-1, 0.05-0.5, 0.15-10, 0.15-2, 0.15-1, or 0.15-0.5.
- the mass ratio of the content of component (C) to the content of component (A2) ((C) component/(A2) component),
- the mass ratio C22 is from the viewpoint that a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer is easily obtained, and the polishing rate of silicon nitride is easily suppressed.
- the mass ratio C22 is 0.01 or more, 0.05 or more, 0.1 or more, 0.15 or more, 0.2 or more, 0.25 or more, 0.3 or more, 0.5 or more, 0.6 or more, It may be 0.65 or greater, 0.7 or greater, 0.8 or greater, 1 or greater, greater than 1, or 1.1 or greater.
- the mass ratio C22 is 10 or less, 8 or less, 5 or less, 2 or less, 1.5 or less, 1.2 or less, 1.1 or less, 1 or less, less than 1, 0.8 or less, 0.7 or less, 0.5 or less.
- the mass ratio C22 is 0.01-10, 0.01-2, 0.01-1, 0.01-0.8, 0.1-10, 0.1-2, 0.01-10. It may be 1 to 1, 0.1 to 0.8, 0.2 to 10, 0.2 to 2, 0.2 to 1, or 0.2 to 0.8.
- the additive of the polishing liquid according to the present embodiment contains, as component (D), a compound having a pH of 3.7 or higher in a 1 mM (millimolar concentration) aqueous solution (excluding compounds corresponding to component (A1)).
- component (D) a compound having a pH of 3.7 or higher in a 1 mM (millimolar concentration) aqueous solution (excluding compounds corresponding to component (A1)).
- component (E) described later can be used as the component (D).
- the interaction between the polishing liquid and the silicon oxide on the protrusions in the pattern of protrusions and recesses is enhanced, thereby making it easier to obtain a high removal rate of the silicon oxide on the protrusions.
- Compounds that can be acid-dissociated in multiple stages have multiple pKa values, and thus it is complicated to select an effective compound based on the pKa values. You can avoid such complications.
- the pH of the 1 mM aqueous solution of component (D) may be within the following ranges from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer.
- the pH of a 1 mM aqueous solution of component (D) is 3.7 or higher, 3.8 or higher, 4.0 or higher, 4.5 or higher, 5.0 or higher, 5.0 or higher, 5.4 or higher, 5.5.
- the pH of the 1 mM aqueous solution of component (D) is 14.0 or less, 13.0 or less, 12.0 or less, 11.0 or less, 10.5 or less, 10.2 or less, 10.0 or less, 9.8.
- the pH of the 1 mM aqueous solution of component (D) is 3.7 to 14.0, 3.7 to 12.0, 3.7 to 11.0, 5.0 to 14.0, 5 .0-12.0, 5.0-11.0, 8.0-14.0, 8.0-12.0, 8.0-11.0, 10.0-14.0, 10.0 ⁇ 12.0, or between 10.0 and 11.0.
- the 1 mM aqueous solution of component (D) is a mixture of component (D) and water.
- Component (D) includes amino acids, pyridine compounds (compounds having a pyridine ring), imidazole compounds (compounds having an imidazole ring), pyrazole compounds (compounds having a pyrazole ring), triazole compounds (compounds having a triazole ring), amino compounds containing a group and a benzene ring, triethanolamine (2,2′,2′′-nitrilotriethanol, etc.), and the like.
- Amino acids include histidine (L-histidine, etc.), lysine, arginine, glutamine (L-glutamine, etc.), glutamic acid (L-glutamic acid, etc.), proline (L-proline, etc.), bicine, cysteine (L-cysteine, etc.), Alanine (L-alanine etc.), serine (L-serine etc.), aminoacetic acid (glycine), tyrosine (L-tyrosine etc.), phenylalanine and the like. Amino acids may be basic amino acids or aromatic amino acids.
- Pyridine compounds include pyridine, hydroxypyridine (3-hydroxypyridine, 4-hydroxypyridine, etc.), pyridinecarboxylic acid (nicotinic acid, picolinic acid, etc.), methylpyridine (2-methylpyridine, etc.), acetylpyridine (2-acetyl pyridine, etc.), pyridineethanol (2-pyridineethanol, etc.), aminopyridine (3-aminopyridine, etc.), and the like.
- Examples of imidazole compounds include imidazole, methylimidazole (2-methylimidazole etc.), dimethylimidazole (1,2-dimethylimidazole etc.) and the like.
- the pyrazole compound includes pyrazole, methylpyrazole and the like.
- Triazole compounds include triazole (1,2,4-triazole, etc.), aminotriazole (3-amino-1,2,4-triazole, etc.), and the like.
- Compounds containing an amino group and a benzene ring include aminobenzene (aniline), anthranilic acid, and the like.
- Component (D) is an amino acid, a pyridine compound, an imidazole compound, a pyrazole compound, a triazole compound, and an amino group from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer. and a compound containing a benzene ring, and at least one selected from the group consisting of triethanolamine, histidine, aminoacetic acid, hydroxypyridine, pyridineethanol, imidazole, methylimidazole, and the group consisting of triethanolamine It may contain at least one selected from.
- the additive of the polishing liquid according to the present embodiment may contain hydroxypyridine or may contain triethanolamine.
- Component (D) is an aromatic polyoxyalkylene compound (having an aromatic ring and a polyoxyalkylene chain) from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer.
- compounds may include compounds that do not have an aromatic ring, and may include compounds that do not have a polyoxyalkylene chain.
- the molecular weight of component (D) may be within the following ranges from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer.
- Component (D) has a molecular weight of 50 or more, 60 or more, 70 or more, 80 or more, 85 or more, 90 or more, 100 or more, 110 or more, 120 or more, 123 or more, 125 or more, 130 or more, 140 or more, 148 or more, Alternatively, it may be 150 or more.
- the molecular weight of component (D) is 1000 or less, less than 1000, 900 or less, 800 or less, 700 or less, 600 or less, 500 or less, 400 or less, 350 or less, 300 or less, 280 or less, 250 or less, less than 250, 240 or less, 230 or less, 210 or less, 200 or less, 180 or less, 170 or less, 160 or less, 150 or less, 148 or less, 140 or less, 130 or less, 125 or less, 123 or less, 120 or less, 110 or less, 100 or less, 90 or less, 85 or less , 80 or less, or 70 or less. From these viewpoints, the molecular weight of component (D) is ⁇ 500, 80-200, or 80-100.
- the content of component (D) is within the following range based on the total mass of the polishing liquid, from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer. you can
- the content of component (D) is 0.001% by mass or more, 0.005% by mass or more, 0.01% by mass or more, 0.015% by mass or more, 0.02% by mass or more, 0.025% by mass or more , 0.03% by mass or more, 0.035% by mass or more, 0.04% by mass or more, 0.05% by mass or more, 0.06% by mass or more, 0.08% by mass or more, 0.1% by mass or more, It may be 0.15% by mass or more, 0.2% by mass or more, or 0.3% by mass or more.
- the content of component (D) is 5% by mass or less, 3% by mass or less, 1% by mass or less, 0.5% by mass or less, 0.4% by mass or less, 0.3% by mass or less, and 0.2% by mass. 0.15% by mass or less, 0.1% by mass or less, 0.08% by mass or less, 0.06% by mass or less, 0.05% by mass or less, 0.04% by mass or less, 0.035% by mass or less , 0.03 mass % or less, 0.025 mass % or less, or 0.02 mass % or less.
- the content of component (D) is 0.01 to 5% by mass, 0.01 to 1% by mass, 0.01 to 0.1% by mass, 0.01 to 0.05% by mass, 0.02-5% by mass, 0.02-1% by mass, 0.02-0.1% by mass, 0.02-0.05% by mass, 0.03-5% by mass, 0.03-1% by mass %, 0.03-0.1% by weight, or 0.03-0.05% by weight.
- the content of component (D) includes the content of compounds corresponding to component (D) and component (E) (the same applies hereinafter).
- the mass ratio D1 of the content of component (D) to the content of abrasive grains (component (D)/abrasive grains) is such that the high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer is From the viewpoint of easy acquisition, the following ranges may be used.
- the mass ratio D1 is 0.001 or more, 0.005 or more, 0.01 or more, 0.05 or more, 0.08 or more, 0.1 or more, 0.11 or more, 0.12 or more, 0.15 or more, It may be 0.16 or greater, 0.2 or greater, 0.3 or greater, 0.5 or greater, 1 or greater, or greater than 1.
- the mass ratio D1 is 10 or less, 5 or less, 2 or less, 1 or less, less than 1, 0.5 or less, 0.3 or less, 0.2 or less, 0.16 or less, 0.15 or less, 0.12 or less, It may be 0.11 or less, 0.1 or less, or 0.08 or less. From these viewpoints, the mass ratio D1 is 0.001 to 10, 0.001 to 1, 0.001 to 0.2, 0.01 to 10, 0.01 to 1, 0.01 to 0.2, It may be from 0.1 to 10, from 0.1 to 1, or from 0.1 to 0.2.
- the mass ratio D2 of the content of component (D) to the content of component (A1) ((D) component/(A1) component) is high in silicon oxide in the convex portions of the pattern wafer relative to silicon oxide in the blanket wafer. From the viewpoint of easily obtaining the polishing speed ratio, the following ranges may be used.
- the mass ratio D2 is 0.01 or more, 0.05 or more, 0.1 or more, 0.3 or more, 0.5 or more, 0.6 or more, 0.8 or more, 0.85 or more, 0.9 or more, It may be 1 or more, more than 1, 1.1 or more, 1.2 or more, 1.4 or more, 1.5 or more, 2 or more, 5 or more, or 8 or more.
- the mass ratio D2 is 10 or less, 8 or less, 5 or less, 2 or less, 1.5 or less, 1.4 or less, 1.2 or less, 1.1 or less, 1 or less, less than 1, 0.9 or less, 0.9 or less. It may be 85 or less, 0.8 or less, or 0.6 or less. From these viewpoints, the mass ratio D2 is 0.01 to 10, 0.01 to 2, 0.01 to 1.2, 0.1 to 10, 0.1 to 2, 0.1 to 1.2, It may be 0.8-10, 0.8-2, or 0.8-1.2.
- Component (E) a cyclic compound having at least one functional group selected from the group consisting of a carboxy group, a carboxylic acid group, an amino group and a hydroxy group
- the additive of the polishing liquid according to the present embodiment may contain component (E) (excluding compounds corresponding to component (A1) or component (A2)).
- component (E) By using the component (E), the interaction between the polishing liquid and the silicon oxide on the protrusions in the pattern of protrusions and recesses is enhanced, thereby making it easier to obtain a high polishing rate for the silicon oxide on the protrusions.
- the component (E) contains at least one selected from the group consisting of a carboxy group and a carboxylic acid group, from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer.
- a compound corresponding to the component (D) can be used.
- Salts of carboxylic acid groups include alkali metal salts such as sodium salts and potassium salts.
- the (E) component can have at least one selected from the group consisting of aromatic rings, heterocyclic rings (excluding aromatic rings) and alicyclic rings.
- the aromatic ring may be a heteroaromatic ring.
- Aromatic rings include benzene ring, naphthalene ring, anthracene ring, pyridine ring, quinoline ring and the like.
- the (E) component may have an aromatic ring different from the benzene ring.
- Component (E) may contain an aromatic compound (a compound having an aromatic ring) from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer. at least one selected from the group consisting of aromatic carboxylic acids (aromatic compounds having a carboxyl group) and aromatic carboxylates (aromatic compounds having a carboxylic acid group).
- Component (E) contains aromatic aminocarboxylic acids (aminobenzoic acid, aminobenzenesulfonic acid, etc.), aromatic oxycarboxylic acids (aromatic hydroxycarboxylic acids, excluding aromatic aminocarboxylic acids), amino groups and hydroxy groups.
- It may contain at least one selected from the group consisting of aromatic carboxylic acids (quinolinecarboxylic acid, pyridinecarboxylic acid, etc.) and salts thereof, aromatic aminocarboxylic acids, quinolinecarboxylic acids, pyridinecarboxylic acids and It may contain at least one selected from the group consisting of these salts.
- Component (E) is benzoic acid, benzoic acid derivatives, hydroxyphenylacetic acid, alkylsalicylic acid, and phthalic acid from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer. , phthalic acid derivatives, quinoline derivatives, pyridine derivatives, aminobenzenesulfonic acid, salts thereof, and salicylaldoxime.
- the benzoic acid derivative contains at least one selected from the group consisting of hydroxybenzoic acid and aminobenzoic acid from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer.
- Hydroxybenzoic acid includes salicylic acid (2-hydroxybenzoic acid), 4-hydroxybenzoic acid and the like. Anthranilic acid etc. are mentioned as amino benzoic acid. Hydroxyphenylacetic acid includes mandelic acid and the like.
- Alkylsalicylic acids include methylsalicylic acid (eg, 3-methylsalicylic acid) and the like.
- the phthalic acid derivative may contain at least one selected from the group consisting of alkylphthalic acid, aminophthalic acid, and sulfophthalic acid.
- Alkyl phthalic acids include methyl phthalic acid (eg, 4-methyl phthalic acid) and the like.
- Aminophthalic acid includes 4-aminophthalic acid and the like.
- Sulfophthalic acid includes 4-sulfophthalic acid and the like.
- the quinoline derivative may contain quinolinecarboxylic acid from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer. Quinaldinic acid etc. are mentioned as a quinoline carboxylic acid.
- the pyridine derivative may contain pyridinecarboxylic acid from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer. Nicotinic acid etc. are mentioned as a pyridine carboxylic acid. Aminobenzenesulfonic acids include altanilic acid and the like.
- Component (E) may be in an embodiment containing at least one selected from the group consisting of quinaldic acid and salts thereof, or in an embodiment containing at least one selected from the group consisting of anthranilic acid and salts thereof.
- Component (E) is a group consisting of aminobenzoic acid, hydroxyphenylacetic acid, quinoline derivatives and pyridine derivatives from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer. It may contain at least one selected from.
- the molecular weight of component (E) may be within the following range from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer.
- Component (E) has a molecular weight of 80 or more, 90 or more, 100 or more, 110 or more, 120 or more, 125 or more, 130 or more, 135 or more, 138 or more, 140 or more, 150 or more, 160 or more, or 170 or more.
- the molecular weight of component (E) is 1000 or less, less than 1000, 900 or less, 800 or less, 700 or less, 600 or less, 500 or less, 400 or less, 300 or less, 250 or less, 200 or less, 180 or less, 170 or less, 160 or less, It may be 150 or less, 140 or less, 138 or less, 135 or less, 130 or less, or 125 or less. From these viewpoints, the molecular weight of component (E) is 80 to 1000, 80 to 200, 80 to 150, 100 to 1000, 100 to 200, 100 to 150, 120 to 1000, 120 to 200, 120 to 150, 130 ⁇ 1000, 130-200, or 130-150.
- the content of component (E) is within the following range based on the total mass of the polishing liquid, from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer. you can
- the content of component (E) is 0.001% by mass or more, 0.005% by mass or more, 0.01% by mass or more, 0.015% by mass or more, 0.02% by mass or more, 0.025% by mass or more , 0.03% by mass or more, 0.035% by mass or more, 0.04% by mass or more, 0.05% by mass or more, 0.06% by mass or more, or 0.08% by mass or more.
- component (E) is 5% by mass or less, 3% by mass or less, 1% by mass or less, 0.5% by mass or less, 0.3% by mass or less, 0.1% by mass or less, and 0.08% by mass. Below, it may be 0.06% by mass or less, 0.05% by mass or less, or 0.04% by mass or less.
- the content of component (E) is 0.001 to 5% by mass, 0.001 to 1% by mass, 0.001 to 0.1% by mass, 0.001 to 0.05% by mass, 0.01 to 5% by mass, 0.01 to 1% by mass, 0.01 to 0.1% by mass, 0.01 to 0.05% by mass, 0.03 to 5% by mass, 0.03 to 1% by mass %, 0.03-0.1% by weight, or 0.03-0.05% by weight.
- the content of component (E) includes the content of compounds corresponding to component (D) and component (E) (the same applies hereinafter).
- the mass ratio E1 of the content of component (E) to the content of abrasive grains ((E) component/abrasive grains) is such that the high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer is From the viewpoint of easy acquisition, the following ranges may be used.
- Mass ratio E1 is 0.01 or more, 0.03 or more, 0.04 or more, 0.05 or more, 0.08 or more, 0.1 or more, 0.12 or more, 0.15 or more, or 0.16 or more.
- Mass ratio E1 is 1 or less, less than 1, 0.8 or less, 0.6 or less, 0.5 or less, 0.4 or less, 0.3 or less, 0.25 or less, 0.2 or less, 0.16 or less , 0.15 or less, 0.12 or less, 0.1 or less, or 0.08 or less. From these viewpoints, the mass ratio E1 is 0.01 to 1, 0.01 to 0.5, 0.01 to 0.2, 0.01 to 0.1, 0.05 to 1, 0.05 to It may be 0.5, 0.05-0.2, 0.05-0.1, 0.1-1, 0.1-0.5, or 0.1-0.2.
- the mass ratio E2 ((E) component/(A1) component) of the content of component (E) to the content of component (A1) is high in silicon oxide in the convex portions of the pattern wafer relative to silicon oxide in the blanket wafer. From the viewpoint of easily obtaining the polishing speed ratio, the following ranges may be used.
- the mass ratio E2 may be 0.1 or more, 0.2 or more, 0.3 or more, 0.4 or more, 0.5 or more, 0.6 or more, 0.8 or more, or 1 or more.
- the mass ratio E2 may be 10 or less, 5 or less, 3 or less, 2 or less, 1.5 or less, 1.2 or less, 1 or less, 0.8 or less, or 0.6 or less. From these viewpoints, the mass ratio E2 is 0.1 to 10, 0.1 to 3, 0.1 to 2, 0.1 to 1, 0.3 to 10, 0.3 to 3, 0.3 to It may be 2, 0.3-1, 1-10, 1-3, or 1-2.
- the additive of the polishing liquid according to the present embodiment may further contain other components (components not corresponding to the above components) in accordance with desired properties.
- components include nonionic polymers; cationic compounds; pH adjusters described later; polar solvents such as ethanol and acetone; and cyclic monocarboxylic acids.
- the polishing liquid according to the present embodiment may contain a compound a having a molecular weight of 100000 or less and having 4 or more hydroxy groups, or may contain no compound a.
- the content of compound a is 0.01% by mass or less, less than 0.01% by mass, 0.001% by mass or less, 0.0001% by mass or less, or substantially 0, based on the total mass of the polishing liquid. % by mass.
- the polishing liquid according to this embodiment may contain the compound b having four or more amino groups, or may not contain the compound b.
- the content of compound b is 0.001% by mass or less, less than 0.001% by mass, 0.0001% by mass or less, 0.00001% by mass or less, or substantially 0, based on the total mass of the polishing liquid. % by mass.
- the mass ratio of the content of compound a to the content of compound b may be 0.10 or less, or less than 0.10.
- Water is not particularly limited, but may contain at least one selected from the group consisting of deionized water, ion-exchanged water and ultrapure water.
- the pH of the polishing liquid according to the present embodiment exceeds 4.0 from the viewpoint that the effect of adding the components contained in the polishing liquid can be easily obtained.
- the pH has a viewpoint that it is easy to suppress the agglomeration of abrasive grains, etc., a viewpoint that a high polishing rate ratio of silicon oxide on the convex part of the pattern wafer to the silicon oxide on the blanket wafer is easily obtained, and a silicon nitride that can be used as a stopper material.
- the pH is 4.1 or more, 4.2 or more, 4.3 or more, 4.4 or more from the viewpoint of easily obtaining a high polishing rate ratio of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer. , 4.5 or more, 4.6 or more, 4.7 or more, 4.8 or more, 5.0 or more, 5.5 or more, 5.5 or more, 6.0 or more, 6.0 or more, 6.5 or more , greater than or equal to 7.0, or greater than 7.0. From these viewpoints, the pH is more than 4.0 and 12.0 or less, more than 4.0 and less than 9.0, more than 4.0 and 8.0 or less, more than 4.0 and 5.5 or less, more than 4.0 and 5.0.
- a pH adjuster may be used to adjust the pH to the above range.
- the pH adjuster is not particularly limited, but examples include acids such as nitric acid, sulfuric acid, hydrochloric acid, phosphoric acid, and boric acid; bases such as sodium hydroxide, ammonia (e.g., aqueous ammonia), potassium hydroxide, and calcium hydroxide; etc.
- the above-mentioned additives such as saturated monocarboxylic acid, aminoacetic acid, etc. may be used for pH adjustment.
- a polishing liquid may be prepared without using a pH adjuster, and this polishing liquid may be applied to CMP as it is.
- the polishing liquid according to the present embodiment can be classified into (a) a normal type, (b) a concentrated type, and (c) a multiple-liquid type (for example, a two-liquid type, polishing liquid set for CMP). Law is different.
- the normal type is a polishing liquid that can be used as it is without pretreatment such as dilution at the time of polishing.
- the (b) concentrated type is a polishing liquid in which the components are concentrated compared to the (a) normal type in consideration of the convenience of storage or transportation.
- Multiple-liquid type is a state in which the components are divided into multiple liquids (for example, a first liquid containing a certain component and a second liquid containing other components) during storage or transportation. It is a polishing liquid that is mixed with these liquids before use.
- the normal type can be obtained by dissolving or dispersing abrasive grains and additives in water, which is the main dispersion medium.
- the blending amount may be adjusted so that 5 g and 1 g of the additive are obtained.
- the polishing liquid can be prepared using, for example, a stirrer, homogenizer, ultrasonic disperser, wet ball mill, and the like.
- the abrasive grains may be finely divided so that the average grain size of the abrasive grains falls within the desired range.
- Abrasive grain micronization can be performed by a sedimentation classification method or a method using a high-pressure homogenizer.
- the sedimentation classification method is a method comprising a step of forcibly sedimenting slurry containing abrasive grains with a centrifuge and a step of taking out only the supernatant liquid.
- the method using a high-pressure homogenizer is a method in which abrasive grains in a dispersion medium collide with each other at high pressure.
- (b) Concentrated type is diluted with water so that the content of the ingredients is the desired content immediately before use. After dilution, (a) liquid characteristics (pH, grain size of abrasive grains, etc.) and polishing characteristics (silicon oxide polishing rate, polishing selectivity between silicon oxide and silicon nitride, etc.) comparable to those of the normal type can be obtained. Stirring may be performed for any length of time up to . In such a (b) concentration type, the volume becomes smaller according to the degree of concentration, so the cost for storage and transportation can be reduced.
- liquid characteristics pH, grain size of abrasive grains, etc.
- polishing characteristics silicon oxide polishing rate, polishing selectivity between silicon oxide and silicon nitride, etc.
- the concentration ratio may be 1.5 times or more, 2 times or more, 3 times or more, or 5 times or more. When the concentration ratio is 1.5 times or more, there is a tendency to obtain advantages in terms of storage and transportation as compared with cases where the concentration ratio is less than 1.5 times.
- the concentration factor may be 40 times or less, 20 times or less, or 15 times or less. When the concentration ratio is 40 times or less, the agglomeration of abrasive grains tends to be suppressed more easily than when the concentration ratio exceeds 40 times.
- the (c) multi-liquid type has the advantage of being able to avoid agglomeration of abrasive grains compared to the (b) concentrated type by appropriately separating each liquid (first liquid, second liquid, etc.). .
- the components contained in each liquid are optional.
- Multi-liquid type (polishing liquid set for CMP) is a polishing liquid set for obtaining a polishing liquid by mixing a first liquid (slurry) and a second liquid (additive liquid).
- the constituent components of the polishing liquid for CMP are stored separately into a first liquid and a second liquid, the first liquid containing abrasive grains and water, and the second liquid containing abrasive grains and water. contains at least one additive and water.
- the first liquid contains abrasive grains and water
- the second liquid is selected from the group consisting of components (A1) and (A2). It contains at least one kind, component (B), and water.
- the first liquid contains abrasive grains, at least one selected from the group consisting of components (A1) and (A2), and water, and the second contains the component (B) and water.
- the first liquid contains abrasive grains, one of the components (A1) and (A2), the component (B), and water
- the second liquid contains the other of the components (A1) and (A2) and water.
- the first liquid contains abrasive grains, the component (B), and water
- the second liquid contains the components (A1) and (A2). At least one selected from the group consisting of and water.
- the first liquid and the second liquid may contain other components blended as necessary.
- any acid or alkali may be added to the first liquid to adjust the pH.
- a multi-liquid type polishing liquid is useful in the case of a combination of components whose polishing properties tend to deteriorate in a relatively short period of time due to aggregation of abrasive grains when mixed.
- the liquids may be of the concentrated type from the viewpoint of cost reduction for storage and transportation.
- each liquid and water may be mixed when using the polishing liquid.
- concentration ratio and pH of each solution are arbitrary, and it is sufficient that the final mixture can have the same level of liquid characteristics and polishing characteristics as (a) the ordinary type of polishing solution.
- the polishing method according to this embodiment includes a polishing step of polishing a surface to be polished using the polishing liquid according to this embodiment.
- the polishing liquid used in the polishing step may be a polishing liquid obtained by mixing the first liquid and the second liquid in the polishing liquid set described above. That is, the polishing method according to the present embodiment may include a polishing step of polishing the surface to be polished using the polishing liquid obtained by mixing the first liquid and the second liquid in the polishing liquid set described above. .
- the polishing method according to the present embodiment uses a polishing liquid in which the content of each component, pH, etc. are adjusted, and can planarize a substrate having a silicon oxide film on its surface by CMP technology.
- the polishing method according to the present embodiment is suitable for polishing that requires high speed, high flatness, and low polishing scratches, such as the polishing of ILD films, and is suitable for polishing many ILD films in a short time. .
- the polishing liquid according to the present embodiment since the polishing liquid according to the present embodiment is used, the occurrence of polishing scratches can be reduced while suppressing the aggregation of abrasive grains and achieving a sufficiently high polishing rate. be able to.
- the polishing step may be a step of supplying the polishing liquid according to the present embodiment between the substrate and a polishing member (polishing member, polishing pad, etc.) and polishing the substrate with the polishing member.
- the polishing method according to this embodiment is suitable for polishing a substrate having a silicon oxide film on its surface. Therefore, the surface to be polished may contain silicon oxide, and in the polishing step, the polishing liquid according to the present embodiment is supplied between the silicon oxide film on the substrate having the silicon oxide film on the surface and the polishing member, and the polishing is performed. It may be a step of polishing the silicon oxide film with a member.
- the surface to be polished may have an uneven pattern composed of convex portions (Line portions) and concave portions (Space portions), and the convex portions may contain silicon oxide.
- the width of the protrusions in the uneven pattern may be 30 ⁇ m or less, or 20 ⁇ m or less.
- the width of the protrusions in the uneven pattern may be 10 ⁇ m or more, or 20 ⁇ m or more.
- the sum of the width of the protrusions and the width of the recesses in the uneven pattern may be 200 ⁇ m or less, or 100 ⁇ m or less.
- the sum of the width of the protrusions and the width of the recesses in the uneven pattern may be 80 ⁇ m or more, or 100 ⁇ m or more.
- the polishing method according to this embodiment is suitable for polishing a substrate having a silicon oxide film on its surface in the device manufacturing process.
- Devices include discrete semiconductors such as diodes, transistors, compound semiconductors, thermistors, varistors, and thyristors; DRAM (dynamic random access memory), SRAM (static random access memory), EPROM (erasable programmable read) memory), mask ROM (mask read only memory), EEPROM (electrically erasable programmable read only memory), flash memory, etc.; logic circuits such as microprocessors, DSPs, ASICs, etc. Devices; integrated circuit devices such as compound semiconductors represented by MMICs (monolithic microwave integrated circuits); hybrid integrated circuits (hybrid ICs); light emitting diodes;
- a high polishing rate can be achieved without greatly depending on the uneven shape of the surface to be polished. Therefore, the polishing method using the polishing liquid can be applied to a substrate for which it is difficult to achieve a high polishing rate with the conventional method using the polishing liquid.
- the polishing method according to the present embodiment is suitable for flattening a surface to be polished having steps (unevennesses) on the surface.
- Substrates having such a polished surface include, for example, logic semiconductor devices.
- the polishing method according to the present embodiment is suitable for polishing a surface including a portion in which concave portions or convex portions are T-shaped or lattice-shaped when viewed from above.
- the polishing method according to the present embodiment can polish a silicon oxide film provided on the surface of a semiconductor device (DRAM, flash memory, etc.) having memory cells at a high speed. For these reasons, it has been difficult to achieve a high polishing rate with a conventional method using a polishing liquid for CMP. It shows that a high polishing rate can be achieved without depending on
- the substrate is not limited to a substrate having only a silicon oxide film on the surface, and may be a substrate having a silicon nitride film, a polycrystalline silicon film, etc. on the surface in addition to the silicon oxide film.
- the substrate is an inorganic insulating film such as silicon oxide, glass, silicon nitride, etc.; a film mainly containing polysilicon, Al, Cu, Ti, TiN, W, Ta, TaN, etc., on a wiring board having predetermined wiring. It may be a substrate having
- FIG. 1 is a schematic cross-sectional view showing the process of polishing an ILD film, showing the process of forming an ILD film between wirings.
- FIG. 1(a) is a schematic cross-sectional view showing a substrate before polishing.
- FIG. 1(b) is a schematic cross-sectional view showing the substrate after polishing.
- a wiring 20 is formed through an ILD film 10 on a lower substrate (not shown) having predetermined lower wiring (not shown).
- a silicon oxide film 30 is formed to cover the wiring 20 . Since the silicon oxide film 30 is formed on the ILD film 10 on which the wirings 20 are formed, the portion above the wirings 20 is higher than the other portion, thereby forming a step on the surface of the silicon oxide film 30 . D is occurring.
- the wiring 20 is connected to lower wiring and the like by a contact plug 40 formed to penetrate the ILD film 10 .
- the partially protruding unnecessary portions on the surface of the silicon oxide film 30 are preferentially removed by CMP.
- the substrate 100 is placed on the polishing member so that the surface of the silicon oxide film 30 and the polishing member are in contact with each other, and the surface of the silicon oxide film 30 is polished by the polishing member. More specifically, the surface to be polished (front surface) side of the silicon oxide film 30 is pressed against the polishing member of the polishing platen, and the polishing liquid is supplied between the surface to be polished and the polishing member while the two are placed relatively to each other.
- the silicon oxide film 30 is polished by moving the .
- step D is eliminated, and finally, as shown in FIG. 1(b), the height of the portion of the wiring 20 on the surface of the silicon oxide film 30 and the height of the other portion become substantially the same, and the surface is flat.
- a substrate 100a having a silicon oxide film 30 (ILD film) having a smooth surface is obtained.
- polishing apparatus used for polishing for example, an apparatus comprising a holder for holding a substrate, a polishing platen to which a polishing pad is attached, and means for supplying polishing liquid onto the polishing pad can be used.
- the polishing device include polishing devices manufactured by Ebara Corporation (model numbers: EPO-111, EPO-222, F-REX200 and F-REX300), and polishing devices manufactured by Applied Materials (trade names: Mirra3400 and Reflexion). be done.
- the constituent material of the polishing pad is not particularly limited, and for example, general non-woven fabric, foamed polyurethane, porous fluororesin, etc. can be used. Further, the polishing pad may be grooved so that the polishing liquid is accumulated.
- the polishing conditions are not particularly limited, but from the viewpoint of preventing the substrate from popping out, the rotational speed of the polishing platen may be 200 min ⁇ 1 or less.
- the pressure (processing load) applied to the substrate may be 100 kPa or less from the viewpoint of easily suppressing scratches on the surface to be polished.
- the polishing liquid may be continuously supplied to the polishing pad by a pump or the like. There is no limit to the amount of supply, but the surface of the polishing pad may always be covered with the polishing liquid. After the polishing is finished, the substrate may be thoroughly washed in running water, and dried after removing water droplets adhering to the substrate using a spin dryer or the like.
- a structure having a desired number of layers can be manufactured by repeating the steps of forming a film and polishing the film a predetermined number of times.
- the substrate (structure) thus obtained can be used as various electronic components.
- electronic components include semiconductor elements; optical glasses such as photomasks, lenses, and prisms; inorganic conductive films such as ITO; optical integrated circuits, optical switching elements, and optical waveguides composed of glass and crystalline materials; optical single crystals such as scintillators; solid laser single crystals; sapphire substrates for blue laser LEDs; semiconductor single crystals such as SiC, GaP and GaAs; magnetic disk glass substrates;
- a method for manufacturing a component according to this embodiment includes a component manufacturing step of obtaining a component using a substrate (member to be polished) that has been polished by a polishing method according to this embodiment.
- a component according to this embodiment is a component obtained by a method for manufacturing a component according to this embodiment.
- the component according to the present embodiment is not particularly limited, but may be an electronic component (for example, a semiconductor component such as a semiconductor package), a wafer (for example, a semiconductor wafer), or a chip (for example, a semiconductor chip). good.
- an electronic component is obtained using a substrate polished by the polishing method according to the present embodiment.
- a semiconductor component for example, a semiconductor package
- the component manufacturing method according to the present embodiment may include a polishing step of polishing the substrate by the polishing method according to the present embodiment before the component manufacturing step.
- the method for manufacturing a component according to the present embodiment may include, as one aspect of the component manufacturing process, a singulation step for singulating the substrate (member to be polished) that has been polished by the polishing method according to the present embodiment.
- the singulation step may be, for example, a step of obtaining chips (eg, semiconductor chips) by dicing a wafer (eg, semiconductor wafer) polished by the polishing method according to the present embodiment.
- the method for manufacturing an electronic component according to the present embodiment includes dividing the substrate polished by the polishing method according to the present embodiment into individual electronic components (for example, semiconductor a step of obtaining a part).
- the method for manufacturing a semiconductor component according to the present embodiment includes dividing a substrate polished by the polishing method according to the present embodiment into individual semiconductor components (for example, semiconductor package).
- the method for manufacturing a component according to the present embodiment connects (for example, electrically connecting).
- the object to be connected to be connected to the substrate polished by the polishing method according to the present embodiment is not particularly limited, and may be the substrate polished by the polishing method according to the present embodiment. It may be an object to be connected that is different from the substrate polished by.
- the connecting step the substrate and the object to be connected may be directly connected (connected while the substrate and the object to be connected are in contact), or the substrate and the object to be connected may be connected via another member (such as a conductive member). You can The connection step can be performed before the singulation step, after the singulation step, or before and after the singulation step.
- the connecting step may be a step of connecting the surface to be polished of the substrate polished by the polishing method according to the present embodiment and the object to be connected, and connecting the substrates polished by the polishing method according to the present embodiment. It may be a step of connecting the surface and the connection surface of the object to be connected.
- the connection surface of the substrate may be a surface to be polished that has been polished by the polishing method according to this embodiment.
- Through the connecting step it is possible to obtain a connecting body comprising a base body and a connected body.
- the connecting step when the connecting surface of the substrate has a metal portion, the object to be connected may be brought into contact with the metal portion.
- the connection surface of the substrate has a metal portion and the connection surface of the object to be connected has a metal portion
- the metal portions may be brought into contact with each other.
- the metal portion may contain copper.
- a device according to the present embodiment includes at least one selected from the group consisting of a substrate polished by the polishing method according to the present embodiment, and parts according to the present embodiment.
- the above-mentioned cerium oxide mixture liquid sent through ultrasonic irradiation was put into four 500 mL polyethylene containers at a rate of 500 g ⁇ 5 g each.
- the cerium oxide mixture in each container was centrifuged for 2 minutes under the condition that the centrifugal force applied to the outer periphery was 500G. After centrifugation, the supernatant fraction of the container was collected to obtain a slurry.
- the slurry contained about 6.0% by weight of cerium oxide particles (abrasive A) on a total weight basis.
- the above-mentioned cerium oxide mixture liquid sent through ultrasonic irradiation was put into four 500 mL polyethylene containers at a rate of 500 g ⁇ 5 g each.
- the cerium oxide mixture in each container was centrifuged for 5 minutes under the condition that the centrifugal force applied to the outer periphery was 1200G. After centrifugation, the supernatant fraction of the container was collected to obtain a slurry.
- the slurry contained about 2.0% by weight of cerium oxide particles (abrasive B) on a total weight basis.
- a sample for particle size measurement was obtained by diluting the slurry with pure water so that the abrasive grain content was 0.25% by mass based on the total mass.
- the average particle size of the abrasive grains was measured using a laser diffraction/scattering particle size distribution analyzer (manufactured by Microtrac BEL Corp., trade name: Microtrac MT3300EXII). , and the average grain size of the abrasive grains B was 120 nm.
- polishing liquid for CMP> By mixing the slurry, each additive and deionized water according to the following procedure, a polishing liquid having the composition (remainder: deionized water) shown in each table below was obtained.
- TBEED means 2,2',2'',2''-ethylenedinitrilotetraethanol
- EDTP means 1,1',1'',1'''-ethylenedi means nitrilotetra-2-propanol.
- Abrasive grains A were used in Examples excluding Examples 21 and 22 and Comparative Examples, and abrasive grains B were used in Examples 21 and 22.
- Each polishing liquid contains acetic acid in a content corresponding to the content of each abrasive grain as the acetic acid mixed during preparation of the slurry. Note that the pH of a 1 mM aqueous solution of acetic acid is less than 5.0.
- an additive solution was obtained by dissolving each additive in deionized water. Next, equal amounts of the slurry and the additive solution were mixed and stirred for 10 minutes to obtain a concentrated polishing liquid storage liquid containing 5.0% by mass of abrasive grains based on the total mass. rice field.
- the polishing liquid storage liquid contains 20 times the amount of abrasive grains and additives as compared to the final abrasive grain content of 0.25% by mass in the polishing liquid. It contains 5 times the amount of abrasive grains and additives to 1.00% by mass.
- polishing liquids of Examples 1 to 17, 21 to 22 and Comparative Examples 1 and 2 were obtained. Further, the polishing liquids of Examples 18 to 20, 23 to 27 and Comparative Example 3 were obtained by diluting the polishing liquid storage liquid 5 times with deionized water.
- the abrasive grain content is 0.25 mass % based on the total mass (for the polishing liquid with the abrasive grain content of 1.00 mass %, the abrasive grain content is adjusted to 0.25 mass %)
- the average grain size of the abrasive grains in the above slurry was the same as the average grain size of the abrasive grains in the slurry.
- ⁇ Zeta potential measurement> An appropriate amount of the polishing liquid was put into "DelsaNano C" (trade name) manufactured by Beckman Coulter, Inc., and the measurement was performed twice at 25°C. The mean value of the indicated zeta potentials was taken as the zeta potential. In each of the examples and comparative examples, the zeta potential of the abrasive grains was positive.
- a silicon oxide film (initial film thickness: 600 nm) with a test pattern (model number: Sematech864, manufactured by Advantech Co., Ltd., ⁇ 200 mm) having an uneven pattern on the surface was prepared.
- the convex portion (Line portion) has an initial step height of 500 nm higher than the concave portion (Space portion).
- a silicon nitride film (initial film thickness: 140 nm) is provided as a film.
- the pattern wafer has a plurality of 20 mm ⁇ 20 mm die units, and a plurality of 4 mm ⁇ 4 mm unit areas within each die unit.
- the pattern wafer has a unit area of 4 mm x 4 mm, and has a pitch of 100 ⁇ m and a Line/Space (L/S) of 10 ⁇ m/90 ⁇ m (convex density: 10%) to 90 ⁇ m/10 ⁇ m (convex density) in increments of 10 ⁇ m. density: 90%).
- L/S Line/Space
- a polishing apparatus (trade name: Mirra 3400, manufactured by Applied Materials) was used to polish the evaluation wafers described above.
- the evaluation wafer described above was set on a holder having a suction pad for attaching a substrate.
- a porous urethane resin polishing pad (K-groove groove, manufactured by DuPont (Dow), model number: IC-1010) was attached to a polishing platen having a diameter of 500 mm.
- the holder was placed on the polishing pad with the surface to be polished of the evaluation wafer facing downward.
- the inner tube pressure, retainer ring pressure and membrane pressure were set to 14 kPa, 21 kPa and 14 kPa, respectively.
- PVA brush polyvinyl alcohol brush
- polishing rate ratio (PTW/BKW) of silicon oxide on the convex portions of the pattern wafer to silicon oxide on the blanket wafer was calculated. Results are shown in each table.
- the film thickness variation was measured at a total of 41 measurement points (20 points on both sides of the center point) including the center point of the wafer and points spaced 5 mm apart from the center point in the diameter direction (20 points on both sides of the center point). The measurement point next to the measurement point 95 mm from the center was 97 mm from the center). At these 41 points, the amount of change in film thickness was measured for a polishing time of 30 seconds, and the average value was obtained as the polishing rate of the blanket wafer.
- the amount of change in film thickness at the convex portion in the region of L/S 20 ⁇ m/80 ⁇ m was measured to obtain the polishing rate of the patterned wafer.
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Abstract
Description
[1]砥粒と、添加剤と、水と、を含有し、前記砥粒がセリウム系粒子を含み、前記添加剤が、(A1)下記一般式(1)で表される4-ピロン系化合物と、(B)飽和モノカルボン酸と、を含み、pHが4.0を超える、CMP用研磨液。
[2]前記(A1)成分が、3-ヒドロキシ-2-メチル-4-ピロン、5-ヒドロキシ-2-(ヒドロキシメチル)-4-ピロン、及び、2-エチル-3-ヒドロキシ-4-ピロンからなる群より選ばれる少なくとも一種を含む、[1]に記載のCMP用研磨液。
[3]前記(A1)成分の含有量が0.001~5質量%である、[1]又は[2]に記載のCMP用研磨液。
[4]前記(B)成分がプロピオン酸を含む、[1]~[3]のいずれか一つに記載のCMP用研磨液。
[5]前記(B)成分の含有量が0.0001~5質量%である、[1]~[4]のいずれか一つに記載のCMP用研磨液。
[6](C)ヒドロキシアルキル基が結合した2以上の窒素原子を有する化合物を更に含有する、[1]~[5]のいずれか一つに記載のCMP用研磨液。
[7]前記(C)成分がエチレンジニトリロテトラエタノールを含む、[6]に記載のCMP用研磨液。
[8]前記(C)成分がエチレンジニトリロテトラプロパノールを含む、[6]又は[7]に記載のCMP用研磨液。
[9]前記添加剤がヒドロキシピリジンを更に含む、[1]~[8]のいずれか一つに記載のCMP用研磨液。
[10]前記添加剤がL-ヒスチジンを更に含む、[1]~[9]のいずれか一つに記載のCMP用研磨液。
[11]pHが8.0以下である、[1]~[10]のいずれか一つに記載のCMP用研磨液。
[12]砥粒と、添加剤と、水と、を含有し、前記砥粒がセリウム系粒子を含み、前記添加剤が、(A2)ピコリン酸と、(B)飽和モノカルボン酸と、を含み、pHが4.0を超える、CMP用研磨液。
[13]前記(A2)成分の含有量が0.001~5質量%である、[12]に記載のCMP用研磨液。
[14]前記(B)成分がプロピオン酸を含む、[12]又は[13]に記載のCMP用研磨液。
[15]前記(B)成分の含有量が0.0001~5質量%である、[12]~[14]のいずれか一つに記載のCMP用研磨液。
[16](C)ヒドロキシアルキル基が結合した2以上の窒素原子を有する化合物を更に含有する、[12]~[15]のいずれか一つに記載のCMP用研磨液。
[17]前記(C)成分がエチレンジニトリロテトラエタノールを含む、[16]に記載のCMP用研磨液。
[18]前記(C)成分がエチレンジニトリロテトラプロパノールを含む、[16]又は[17]に記載のCMP用研磨液。
[19]pHが8.0以下である、[12]~[18]のいずれか一つに記載のCMP用研磨液。
[20][1]~[19]のいずれか一つに記載のCMP用研磨液の構成成分が第1の液と第2の液とに分けて保存され、前記第1の液が、前記砥粒と、水と、を含み、前記第2の液が、前記添加剤の少なくとも一種と、水と、を含む、CMP用研磨液セット。
[21][1]~[19]のいずれか一つに記載のCMP用研磨液、又は、[20]に記載のCMP用研磨液セットにおける前記第1の液と前記第2の液とを混合して得られるCMP用研磨液を用いて被研磨面を研磨する工程を備える、研磨方法。
[22]前記被研磨面が酸化ケイ素を含む、[21]に記載の研磨方法。
本実施形態(第1実施形態及び第2実施形態。以下同様)に係るCMP用研磨液は、砥粒と、添加剤と、水と、を含有するCMP用研磨液(以下、場合により、単に「研磨液」という)である。砥粒は、セリウム系粒子(セリウム系化合物を含む粒子)を含む。第1実施形態に係る研磨液の添加剤は、(A1)下記一般式(1)で表される4-ピロン系化合物((A1)成分)と、(B)飽和モノカルボン酸((B)成分)と、を含む。第2実施形態に係る研磨液の添加剤は、(A2)ピコリン酸((A2)成分)と、(B)飽和モノカルボン酸((B)成分)と、を含む。本実施形態に係る研磨液の添加剤は、(A1)成分、(A2)成分及び(B)成分を含んでよい。本実施形態に係るCMP用研磨液のpHは、4.0を超える。
砥粒は、セリウム系粒子を含む。セリウム系粒子を砥粒として用いることにより、被研磨面に生じる研磨傷を低減しつつパターンウエハの凸部における酸化ケイ素の高い研磨速度を得やすい。
[(A1)成分:4-ピロン系化合物]
第1実施形態に係る研磨液の添加剤は、(A1)成分として、一般式(1)で表される4-ピロン系化合物(以下、場合により、単に「4-ピロン系化合物」という)を含む。4-ピロン系化合物を用いることで、研磨液と酸化ケイ素との相互作用が大きくなることにより研磨速度が高くなりやすいと推測される。また、4-ピロン系化合物は、研磨液と酸化ケイ素との相互作用を大きくし得る添加剤であるにもかかわらず、砥粒同士の静電的反発力等の反発力を弱める効果がないため、砥粒の凝集を抑制することができると考えられる。
第2実施形態に係る研磨液の添加剤は、(A2)成分として、ピコリン酸を含む。(A2)成分を用いることで、研磨液と酸化ケイ素との相互作用が大きくなることにより研磨速度が高くなりやすいと推測される。
本実施形態に係る研磨液の添加剤は、(B)成分として、飽和モノカルボン酸を含む。(B)成分は、砥粒の分散性の向上等の目的で用いることができる。(B)成分は、ブランケットウエハにおける酸化ケイ素に対するパターンウエハの凸部における酸化ケイ素の研磨速度比、ストッパ材料として使用可能な窒化ケイ素の研磨速度等の調整に寄与することもできる。
本実施形態に係る研磨液の添加剤は、(C)成分として、ヒドロキシアルキル基が結合した2以上の窒素原子を有する化合物(窒素含有ヒドロキシアルキル化合物;但し、(A1)成分に該当する化合物を除く)を含んでよい。(C)成分を用いることにより、研磨液と凹凸パターンにおける凸部の酸化ケイ素との相互作用を大きくすることにより凸部の酸化ケイ素の高い研磨速度を得やすいと共に、ストッパ材料として使用可能な窒化ケイ素の研磨速度を抑制しやすい。(C)成分では、窒素原子にヒドロキシアルキル基が直接結合しており、窒素原子に直接結合したアルキル基にヒドロキシ基が直接結合している。(C)成分は、窒素原子に結合したヒドロキシアルキル基として、ヒドロキシ基以外の置換基を有しないアルキル基を用いることができる。
本実施形態に係る研磨液の添加剤は、(D)成分として、1mM(ミリモル濃度)の水溶液のpHが3.7以上の化合物(但し、(A1)成分に該当する化合物を除く)を含んでよい。(D)成分としては、後述の(E)成分にも該当する化合物を用いることができる。(D)成分を用いることにより、研磨液と凹凸パターンにおける凸部の酸化ケイ素との相互作用を大きくすることにより凸部の酸化ケイ素の高い研磨速度を得やすい。複数段階で酸解離可能な化合物は複数のpKaを有するため、pKaに基づいて有効な化合物を選定することが煩雑であるものの、化合物が1mMの水溶液において与えるpHに基づき化合物を選定することでこのような煩雑さを回避できる。
本実施形態に係る研磨液の添加剤は、(E)成分(但し、(A1)成分又は(A2)成分に該当する化合物を除く)を含んでよい。(E)成分を用いることにより、研磨液と凹凸パターンにおける凸部の酸化ケイ素との相互作用を大きくすることにより凸部の酸化ケイ素の高い研磨速度を得やすい。(E)成分は、ブランケットウエハにおける酸化ケイ素に対してパターンウエハの凸部における酸化ケイ素の高い研磨速度比が得られやすい観点から、カルボキシ基及びカルボン酸塩基からなる群より選ばれる少なくとも一種を有してよい。(E)成分としては、(D)成分にも該当する化合物を用いることができる。カルボン酸塩基の塩としては、ナトリウム塩、カリウム塩等のアルカリ金属塩などが挙げられる。
本実施形態に係る研磨液の添加剤は、所望とする特性に合わせて他の成分(上述の各成分に該当しない成分)を更に含んでよい。このような成分としては、非イオン性ポリマ;カチオン性化合物;後述するpH調整剤;エタノール、アセトン等の極性溶媒;環状モノカルボン酸などが挙げられる。
水は、特に制限されるものではないが、脱イオン水、イオン交換水及び超純水からなる群より選ばれる少なくとも一種を含んでよい。
本実施形態に係る研磨液のpHは、研磨液の含有成分の添加効果が得られやすいこと等の観点から、4.0を超える。pHは、砥粒の凝集等を抑制しやすい観点、ブランケットウエハにおける酸化ケイ素に対してパターンウエハの凸部における酸化ケイ素の高い研磨速度比が得られやすい観点、ストッパ材料として使用可能な窒化ケイ素の研磨速度を抑制しやすい観点、及び、上記添加剤を添加した効果が得られやすい観点から、12.0以下、11.0以下、10.5以下、10.5未満、10.0以下、10.0未満、9.5以下、9.0以下、9.0未満、8.5以下、8.0以下、8.0未満、7.5以下、7.0以下、7.0未満、6.5以下、6.0以下、6.0未満、5.5以下、5.5未満、5.0以下、4.8以下、4.7以下、4.6以下、4.5以下、4.4以下、4.3以下、4.2以下、又は、4.1以下であってよい。pHは、ブランケットウエハにおける酸化ケイ素に対してパターンウエハの凸部における酸化ケイ素の高い研磨速度比が得られやすい観点から、4.1以上、4.2以上、4.3以上、4.4以上、4.5以上、4.6以上、4.7以上、4.8以上、5.0以上、5.5以上、5.5超、6.0以上、6.0超、6.5以上、7.0以上、又は、7.0超であってよい。これらの観点から、pHは、4.0超12.0以下、4.0超9.0未満、4.0超8.0以下、4.0超5.5以下、4.0超5.0以下、4.3~12.0、4.3以上9.0未満、4.3~8.0、4.3~5.5、4.3~5.0、4.5~12.0、4.5以上9.0未満、4.5~8.0、4.5~5.5、又は、4.5~5.0であってよい。pHは、実施例に記載の方法により測定できる。
本実施形態に係る研磨液は、(a)通常タイプ、(b)濃縮タイプ及び(c)複数液タイプ(例えば2液タイプ。CMP用研磨液セット)に分類でき、タイプによってそれぞれ調製法及び使用法が相違する。(a)通常タイプは、研磨時に希釈等の前処理をせずにそのまま使用できる研磨液である。(b)濃縮タイプは、保管又は輸送の利便性を考慮し、(a)通常タイプと比較して含有成分を濃縮した研磨液である。(c)複数液タイプは、保管時又は輸送時には、含有成分を複数の液に分けた状態(例えば、一定の成分を含む第1の液と、他の成分を含む第2の液とに分けた状態)としておき、使用に際してこれらの液を混合して使用する研磨液である。
本実施形態に係る研磨方法は、本実施形態に係る研磨液を用いて被研磨面を研磨する研磨工程を含む。研磨工程で用いられる研磨液は、上述の研磨液セットにおける第1の液と第2の液とを混合して得られる研磨液であってもよい。すなわち、本実施形態に係る研磨方法は、上述の研磨液セットにおける第1の液と第2の液とを混合して得られる研磨液を用いて被研磨面を研磨する研磨工程を含んでよい。
本実施形態に係る部品の製造方法は、本実施形態に係る研磨方法により研磨された基体(被研磨部材)を用いて部品を得る部品作製工程を備える。本実施形態に係る部品は、本実施形態に係る部品の製造方法により得られる部品である。本実施形態に係る部品は、特に限定されないが、電子部品(例えば、半導体パッケージ等の半導体部品)であってよく、ウエハ(例えば半導体ウエハ)であってよく、チップ(例えば半導体チップ)であってよい。本実施形態に係る部品の製造方法の一態様として、本実施形態に係る電子部品の製造方法では、本実施形態に係る研磨方法により研磨された基体を用いて電子部品を得る。本実施形態に係る部品の製造方法の一態様として、本実施形態に係る半導体部品の製造方法では、本実施形態に係る研磨方法により研磨された基体を用いて半導体部品(例えば半導体パッケージ)を得る。本実施形態に係る部品の製造方法は、部品作製工程の前に、本実施形態に係る研磨方法により基体を研磨する研磨工程を備えてよい。
炭酸セリウム水和物40kgをアルミナ製容器10個に分けて入れ、それぞれ830℃で2時間、空気中で焼成して黄白色の粉末を計20kg得た。この粉末についてX線回折法で相同定を行い、当該粉末が多結晶体の酸化セリウムを含むことを確認した。焼成によって得られた粉末の粒径をSEMで観察したところ、20~100μmの範囲であった。次いで、ジェットミルを用いて酸化セリウム粉末20kgの乾式粉砕を行うことにより酸化セリウム粉末を得た。粉砕後の酸化セリウム粉末の比表面積は9.4m2/gであった。比表面積の測定はBET法によって実施した。
上記で得られた酸化セリウム粉末15.0kg及び脱イオン水84.5kgを容器内に入れて混合した。次に、1M(mol/L、約6質量%)の酢酸を0.5kg添加した後、10分間撹拌することにより酸化セリウム混合液を得た。この酸化セリウム混合液を別の容器に30分かけて送液した。その間、送液する配管内で、酸化セリウム混合液に対して超音波周波数400kHzにて超音波照射を行った。
上述のスラリ、各添加剤及び脱イオン水を下記の手順で混合することにより、下記各表の組成(残部:脱イオン水)を有する研磨液を得た。表中、「THEED」は2,2’,2’’,2’’’-エチレンジニトリロテトラエタノールを意味し、「EDTP」は1,1’,1’’,1’’’-エチレンジニトリロテトラ-2-プロパノールを意味する。実施例21及び22を除く実施例、及び、比較例において砥粒Aを用い、実施例21及び22において砥粒Bを用いた。各研磨液は、上述のスラリの調製時に混合した酢酸として、それぞれの砥粒含有量に応じた含有量の酢酸を含有している。なお、酢酸の1mMの水溶液のpHは5.0未満である。
ベックマン・コールター株式会社製の商品名「DelsaNano C」内に適量の研磨液を投入し、25℃において測定を2回行った。表示されたゼータ電位の平均値をゼータ電位として得た。実施例及び比較例のそれぞれにおいて、砥粒のゼータ電位は正であった。
(研磨液のpH)
下記の条件で研磨液のpHを測定した。結果を各表に示す。
測定温度:25℃
測定装置:株式会社堀場製作所の商品名:Model(D-71)
測定方法:フタル酸塩pH標準液(pH:4.01)と、中性リン酸塩pH標準液(pH:6.86)と、ホウ酸塩pH標準液(pH:9.18)とをpH標準液として用いてpHメーターを3点校正した後、pHメーターの電極を研磨液に入れて、2min以上経過して安定した後のpHを前記測定装置により測定した。
下記化合物のそれぞれを脱イオン水に溶解することにより1mM(ミリモル濃度)の溶解液を調製した。研磨液のpHと同様の手順で溶解液のpHを測定した。各化合物の1mM溶液のpHは、下記のとおりであった。
アミノ酢酸:5.9
L-ヒスチジン:7.5
3-ヒドロキシピリジン:6.7
4-ヒドロキシピリジン:6.2
2-ピリジンエタノール:7.2
2-メチルイミダゾール:9.2
イミダゾール:8.6
トリエタノールアミン:9.4
(評価用ウエハの準備)
ブランケットウエハ(BKW)として、表面に酸化ケイ素膜(SiO2、初期膜厚:1000nm)を有するφ200mmのパターン無しのウエハと、表面に窒化ケイ素膜(SiN、初期膜厚:200nm)を有するφ200mmのパターン無しのウエハと、を準備した。
研磨装置(アプライドマテリアル製、商品名:Mirra3400)を用いて上述の評価用ウエハを研磨した。基体取り付け用の吸着パッドを有するホルダーに上述の評価用ウエハをセットした。直径500mmの研磨定盤に多孔質ウレタン樹脂製の研磨パッド(K-groove溝、DuPont(Dow)社製、型番:IC-1010)を貼り付けた。
光干渉式膜厚測定装置(ナノメトリクス・ジャパン株式会社製、商品名:AFT-5100)を用いて下記のとおり研磨前後の被研磨膜の膜厚変化量を測定し、研磨速度を得た。また、ブランケットウエハにおける酸化ケイ素に対するパターンウエハの凸部における酸化ケイ素の研磨速度比(PTW/BKW)を算出した。結果を各表に示す。
Claims (24)
- 前記(A1)成分が、3-ヒドロキシ-2-メチル-4-ピロン、5-ヒドロキシ-2-(ヒドロキシメチル)-4-ピロン、及び、2-エチル-3-ヒドロキシ-4-ピロンからなる群より選ばれる少なくとも一種を含む、請求項1に記載のCMP用研磨液。
- 前記(A1)成分の含有量が0.001~5質量%である、請求項1に記載のCMP用研磨液。
- 前記(B)成分がプロピオン酸を含む、請求項1に記載のCMP用研磨液。
- 前記(B)成分の含有量が0.0001~5質量%である、請求項1に記載のCMP用研磨液。
- (C)ヒドロキシアルキル基が結合した2以上の窒素原子を有する化合物を更に含有する、請求項1に記載のCMP用研磨液。
- 前記(C)成分がエチレンジニトリロテトラエタノールを含む、請求項6に記載のCMP用研磨液。
- 前記(C)成分がエチレンジニトリロテトラプロパノールを含む、請求項6に記載のCMP用研磨液。
- 前記添加剤がヒドロキシピリジンを更に含む、請求項1に記載のCMP用研磨液。
- 前記添加剤がL-ヒスチジンを更に含む、請求項1に記載のCMP用研磨液。
- pHが8.0以下である、請求項1に記載のCMP用研磨液。
- 砥粒と、添加剤と、水と、を含有し、
前記砥粒がセリウム系粒子を含み、
前記添加剤が、(A2)ピコリン酸と、(B)飽和モノカルボン酸と、を含み、
pHが4.0を超える、CMP用研磨液。 - 前記(A2)成分の含有量が0.001~5質量%である、請求項12に記載のCMP用研磨液。
- 前記(B)成分がプロピオン酸を含む、請求項12に記載のCMP用研磨液。
- 前記(B)成分の含有量が0.0001~5質量%である、請求項12に記載のCMP用研磨液。
- (C)ヒドロキシアルキル基が結合した2以上の窒素原子を有する化合物を更に含有する、請求項12に記載のCMP用研磨液。
- 前記(C)成分がエチレンジニトリロテトラエタノールを含む、請求項16に記載のCMP用研磨液。
- 前記(C)成分がエチレンジニトリロテトラプロパノールを含む、請求項16に記載のCMP用研磨液。
- pHが8.0以下である、請求項12に記載のCMP用研磨液。
- 請求項1~19のいずれか一項に記載のCMP用研磨液の構成成分が第1の液と第2の液とに分けて保存され、前記第1の液が、前記砥粒と、水と、を含み、前記第2の液が、前記添加剤の少なくとも一種と、水と、を含む、CMP用研磨液セット。
- 請求項1~19のいずれか一項に記載のCMP用研磨液を用いて被研磨面を研磨する工程を備える、研磨方法。
- 前記被研磨面が酸化ケイ素を含む、請求項21に記載の研磨方法。
- 請求項20に記載のCMP用研磨液セットにおける前記第1の液と前記第2の液とを混合して得られるCMP用研磨液を用いて被研磨面を研磨する工程を備える、研磨方法。
- 前記被研磨面が酸化ケイ素を含む、請求項23に記載の研磨方法。
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JP (3) | JPWO2023013695A1 (ja) |
KR (3) | KR20240027827A (ja) |
CN (3) | CN117751432A (ja) |
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WO2023013692A1 (ja) | 2023-02-09 |
CN117751432A (zh) | 2024-03-22 |
KR20240027830A (ko) | 2024-03-04 |
CN117751431A (zh) | 2024-03-22 |
TW202313923A (zh) | 2023-04-01 |
EP4379776A1 (en) | 2024-06-05 |
JPWO2023013683A1 (ja) | 2023-02-09 |
EP4379778A1 (en) | 2024-06-05 |
TW202321390A (zh) | 2023-06-01 |
JPWO2023013695A1 (ja) | 2023-02-09 |
WO2023013059A1 (ja) | 2023-02-09 |
KR20240024993A (ko) | 2024-02-26 |
KR20240027827A (ko) | 2024-03-04 |
TW202313924A (zh) | 2023-04-01 |
CN117751430A (zh) | 2024-03-22 |
WO2023013683A1 (ja) | 2023-02-09 |
EP4379777A1 (en) | 2024-06-05 |
JPWO2023013692A1 (ja) | 2023-02-09 |
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