WO2017169743A1 - Composition de polissage utilisée pour le polissage d'un objet de polissage ayant une couche qui contient du métal - Google Patents
Composition de polissage utilisée pour le polissage d'un objet de polissage ayant une couche qui contient du métal Download PDFInfo
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- WO2017169743A1 WO2017169743A1 PCT/JP2017/010224 JP2017010224W WO2017169743A1 WO 2017169743 A1 WO2017169743 A1 WO 2017169743A1 JP 2017010224 W JP2017010224 W JP 2017010224W WO 2017169743 A1 WO2017169743 A1 WO 2017169743A1
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- WO
- WIPO (PCT)
- Prior art keywords
- polishing
- polishing composition
- acid
- metal
- group
- Prior art date
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- 238000005498 polishing Methods 0.000 title claims abstract description 295
- 239000000203 mixture Substances 0.000 title claims abstract description 155
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 93
- 239000002184 metal Substances 0.000 title claims abstract description 93
- 239000006061 abrasive grain Substances 0.000 claims abstract description 66
- 125000000524 functional group Chemical group 0.000 claims abstract description 55
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 44
- 239000007800 oxidant agent Substances 0.000 claims abstract description 35
- 230000002378 acidificating effect Effects 0.000 claims abstract description 33
- 239000002612 dispersion medium Substances 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 28
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 28
- 229910052721 tungsten Inorganic materials 0.000 claims description 28
- 239000010937 tungsten Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 23
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 18
- 150000001875 compounds Chemical class 0.000 claims description 17
- 238000004519 manufacturing process Methods 0.000 claims description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 15
- 125000004432 carbon atom Chemical group C* 0.000 claims description 11
- 125000000217 alkyl group Chemical group 0.000 claims description 9
- 150000001412 amines Chemical class 0.000 claims description 9
- KFSLWBXXFJQRDL-UHFFFAOYSA-N Peracetic acid Chemical compound CC(=O)OO KFSLWBXXFJQRDL-UHFFFAOYSA-N 0.000 claims description 8
- 150000002978 peroxides Chemical group 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 239000003002 pH adjusting agent Substances 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 5
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium peroxydisulfate Substances [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 5
- VAZSKTXWXKYQJF-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)OOS([O-])=O VAZSKTXWXKYQJF-UHFFFAOYSA-N 0.000 claims description 5
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 5
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 5
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 5
- 239000012425 OXONE® Substances 0.000 claims description 4
- HJKYXKSLRZKNSI-UHFFFAOYSA-I pentapotassium;hydrogen sulfate;oxido sulfate;sulfuric acid Chemical compound [K+].[K+].[K+].[K+].[K+].OS([O-])(=O)=O.[O-]S([O-])(=O)=O.OS(=O)(=O)O[O-].OS(=O)(=O)O[O-] HJKYXKSLRZKNSI-UHFFFAOYSA-I 0.000 claims description 4
- 125000001453 quaternary ammonium group Chemical group 0.000 claims description 4
- MWNQXXOSWHCCOZ-UHFFFAOYSA-L sodium;oxido carbonate Chemical compound [Na+].[O-]OC([O-])=O MWNQXXOSWHCCOZ-UHFFFAOYSA-L 0.000 claims description 4
- AQLJVWUFPCUVLO-UHFFFAOYSA-N urea hydrogen peroxide Chemical compound OO.NC(N)=O AQLJVWUFPCUVLO-UHFFFAOYSA-N 0.000 claims description 4
- 125000002947 alkylene group Chemical group 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 2
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- 150000003839 salts Chemical class 0.000 description 13
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- 238000000227 grinding Methods 0.000 description 11
- 229920000642 polymer Polymers 0.000 description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 150000005215 alkyl ethers Chemical class 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
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- 239000000126 substance Substances 0.000 description 8
- 239000000654 additive Substances 0.000 description 7
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 7
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- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 5
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- 239000004254 Ammonium phosphate Substances 0.000 description 4
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 125000004103 aminoalkyl group Chemical group 0.000 description 4
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 4
- 235000019289 ammonium phosphates Nutrition 0.000 description 4
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- 125000002091 cationic group Chemical group 0.000 description 4
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- 239000011630 iodine Substances 0.000 description 4
- 229910052740 iodine Inorganic materials 0.000 description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 4
- 239000011976 maleic acid Substances 0.000 description 4
- 238000007517 polishing process Methods 0.000 description 4
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- 230000001681 protective effect Effects 0.000 description 4
- FSYKKLYZXJSNPZ-UHFFFAOYSA-N sarcosine Chemical compound C[NH2+]CC([O-])=O FSYKKLYZXJSNPZ-UHFFFAOYSA-N 0.000 description 4
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- 238000012360 testing method Methods 0.000 description 4
- PZOUSPYUWWUPPK-UHFFFAOYSA-N 4-methyl-1h-indole Chemical compound CC1=CC=CC2=C1C=CN2 PZOUSPYUWWUPPK-UHFFFAOYSA-N 0.000 description 3
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- KWYNZJCVSLOTCZ-UHFFFAOYSA-N P(=O)([O-])([O-])[O-].[NH4+].C(CCCCCCCCCC(C)C)OCCCCCCCCCCC(C)C.[NH4+].[NH4+] Chemical compound P(=O)([O-])([O-])[O-].[NH4+].C(CCCCCCCCCC(C)C)OCCCCCCCCCCC(C)C.[NH4+].[NH4+] KWYNZJCVSLOTCZ-UHFFFAOYSA-N 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 3
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- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
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- JLKDVMWYMMLWTI-UHFFFAOYSA-M potassium iodate Chemical compound [K+].[O-]I(=O)=O JLKDVMWYMMLWTI-UHFFFAOYSA-M 0.000 description 3
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- 125000003396 thiol group Chemical group [H]S* 0.000 description 3
- QWENRTYMTSOGBR-UHFFFAOYSA-N 1H-1,2,3-Triazole Chemical compound C=1C=NNN=1 QWENRTYMTSOGBR-UHFFFAOYSA-N 0.000 description 2
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- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 description 1
- BDPNSNXYBGIFIE-UHFFFAOYSA-J tungsten;tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[W] BDPNSNXYBGIFIE-UHFFFAOYSA-J 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
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
- 239000004474 valine Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
Definitions
- the present invention relates to a polishing composition used for polishing a polishing object having a layer containing a metal.
- CMP chemical mechanical polishing
- a metal plug or a wiring in a semiconductor device is formed by forming a conductor layer made of a metal as described above on an insulator layer made of silicon oxide having a recess and then forming a conductor layer on the insulator layer. This is done by removing a portion by polishing until the insulator layer is exposed.
- This polishing process is roughly divided into a main polishing process for performing polishing for removing most of the conductor layer to be removed, and a buff polishing process for final polishing of the conductor layer and the insulator layer.
- a general method of CMP is to apply a polishing pad on a circular polishing platen (platen), immerse the surface of the polishing pad with a polishing composition, and press the surface on which the metal film of the substrate is formed.
- a polishing platen is rotated with a predetermined pressure (polishing pressure) applied, and the metal film (for example, tungsten) is removed by mechanical friction between the polishing composition and the metal film.
- the action of chemical components contained in the polishing composition increases the mechanical polishing effect due to the relative movement of the polishing composition and the object to be polished, and a high-speed and smooth polishing surface can be obtained.
- a polishing composition used in a semiconductor device manufacturing process generally contains a polishing accelerator such as an acid, an oxidizing agent, and abrasive grains.
- a polishing accelerator such as an acid, an oxidizing agent, and abrasive grains.
- the present invention has been made in view of the above circumstances, and an object thereof is to provide a polishing composition used for polishing an object to be polished having a metal-containing layer that can achieve sufficient planarization.
- Another object of the present invention is to provide a polishing composition used for polishing an object to be polished having a metal-containing layer capable of ensuring a low etching rate and a high polishing rate in a well-balanced manner.
- the present inventors have conducted intensive research to solve the above problems. As a result, the inventors found that the above problems can be solved by using an anticorrosive agent having an acidic functional group and a basic functional group in the composition, and completed the present invention.
- a polishing composition used for polishing a polishing object having a layer containing a metal comprising abrasive grains, an oxidizing agent, a dispersion medium, and an anticorrosive having an acidic functional group and a basic functional group Composition.
- polishing composition according to 1 or 2 wherein the anticorrosive has an acid value of 5 to 150 mgKOH / g and an amine value of 5 to 150 mgKOH / g.
- the anticorrosive agent has the following formula (1):
- R 1 and R 2 are each independently a hydrogen atom or a substituted or unsubstituted linear or branched alkyl group having 8 to 16 carbon atoms
- Y 1 and Y 2 are each independently a single bond or a group represented by the following formula (i)
- at least one of Y 1 and Y 2 is a group represented by the following formula (i);
- R 3 is an alkylene group having 2 to 6 carbon atoms, a plurality of R 3 may be the same or different, n is an integer of 2 to 200, and * is Represents a position bonded to R 1 or R 2 in formula (1), X + is an ammonium ion, a primary ammonium ion, a secondary ammonium ion, a tertiary ammonium ion, or a quaternary ammonium ion;
- the polishing composition according to any one of 1 to 3, which is a compound represented by:
- polishing composition according to any one of 1 to 4, wherein the oxidizing agent is a peroxide.
- the peroxide is at least one selected from the group consisting of hydrogen peroxide, peracetic acid, percarbonate, urea peroxide, sodium persulfate, potassium persulfate, ammonium persulfate, potassium monopersulfate and oxone. 5.
- Polishing method of polishing a polishing object having a metal-containing layer with the polishing composition according to any one of 10.1 to 8.
- a method for manufacturing a substrate including a step of polishing by the polishing method described in 11.10.
- a polishing composition used for polishing an object to be polished having a metal-containing layer according to the present invention includes abrasive grains, an oxidizing agent, a dispersion medium, and an anticorrosive having an acidic functional group and a basic functional group. Polishing composition. According to the polishing composition having the above configuration, a polishing object having a metal-containing layer can be polished smoothly. In addition, according to the polishing composition of the present invention, a polishing object having a metal-containing layer that is a polishing object can be polished at a high polishing rate while keeping the etching rate low.
- polishing composition used for polishing an object to be polished having a metal-containing layer is also simply referred to as “polishing composition according to the present invention” or “polishing composition”.
- the “polishing object having a metal-containing layer” is also simply referred to as “metal polishing object”.
- the composition of the above-mentioned JP2013-42131A includes a diquaternary compound of the formula (I) comprising a divalent cation moiety and a divalent anion moiety (for example, a quaternary amine described in paragraph "0029") Compound). Due to the presence of the diquaternary compound, the etching rate of tungsten can be kept low. However, since the cation portion of the diquaternary compound is adsorbed on the surface of the abrasive grains (for example, Si ⁇ ) and induces aggregation and settling of the abrasive grains, the stability of the abrasive grains decreases.
- a diquaternary compound of the formula (I) comprising a divalent cation moiety and a divalent anion moiety (for example, a quaternary amine described in paragraph "0029") Compound). Due to the presence of the diquaternary compound, the etching rate of tungsten can be kept low. However
- JP 2013-42131 A cannot sufficiently achieve the flatness of the polishing object currently required.
- potassium iodate is essential as an oxidizing agent, and this oxidizing agent promotes the formation of a metal oxide film (for example, a tungsten oxide (WO 3 ) film).
- a metal oxide film for example, a tungsten oxide (WO 3 ) film.
- the potassium iodate causes iodine gas to be generated. Iodine gas induces coughing, wheezing, breathing difficulty, etc. when inhaled by humans.
- ventilation should be sufficient, and workers should wear protective gloves and protective clothing. It is necessary to strictly manage the work environment, such as the need to wear an iron, and in view of the health of the work environment in recent years, it is desirable not to use compounds containing iodine as much as possible.
- the present invention is characterized by using an anticorrosive agent having an acidic functional group and a basic functional group in the composition.
- a polishing object having a metal-containing layer can be polished smoothly (low surface roughness (RMS)) without using the diquaternary compound.
- RMS surface roughness
- a polishing object having a metal-containing layer can be polished at a high polishing rate while keeping the etching rate low.
- CMP chemical mechanical polishing
- the metal oxide film is polished by being physically scraped by abrasive grains, and the polished metal surface is also oxidized by an oxidizing agent to form a metal oxide film, and the metal oxide film is scraped by abrasive grains. Repeat the cycle.
- the conventional method has a problem that the substrate surface after polishing does not have sufficient smoothness.
- the inventors of the present invention have made extensive studies on the above problems, and have estimated that the corrosion of the grain boundary between crystal grains is the cause of the decrease in the surface roughness.
- the rate of dissolution by this chemical reaction is faster than scraping with abrasive grains. It can be presumed that the etching rate increases and surface roughness occurs.
- increasing the scraping speed with abrasive grains has been studied as one of the means for solving the problem, but it is necessary to increase the abrasive grain concentration, and the practicality is low due to high cost.
- the present inventors have intensively studied other means for suppressing the dissolution, that is, the etching rate, and use an anticorrosive having an acidic functional group and a basic functional group in the polishing composition.
- the anticorrosive having an acidic functional group (anionic functional group) and a basic functional group (cationic functional group) is adsorbed on the surface of a metal oxide (eg, tungsten oxide) and covers the metal oxide.
- a metal oxide eg, tungsten oxide
- An etching-inhibiting film is formed on the surface to suppress dissolution of the metal oxide.
- a cationic anticorrosive agent of a diquaternary compound as disclosed in JP2013-42131A when a cationic anticorrosive agent of a diquaternary compound as disclosed in JP2013-42131A is used, the zeta potential on the surface of the abrasive grains (for example, Si ⁇ ) is negatively charged.
- the agent tends to be adsorbed on the surface of the abrasive grains, and a large amount of the anticorrosive agent must be used to obtain a good anticorrosive effect.
- a high concentration of the anticorrosive agent when a high concentration of the anticorrosive agent is used, it causes aggregation and further sedimentation of the abrasive grains. There is.
- the anticorrosive agent according to the present invention has a cationic basic functional group and an anionic acidic functional group, and the cationic functional group is adsorbed to the metal oxide, and at the same time, the anionic functional group is also self-organized. Therefore, a relatively small amount of anticorrosive agent can be used to form a film on the surface of the metal oxide without causing agglomeration of the abrasive grains, and the etching rate can be suppressed. .
- a metal-containing layer (polishing object) can be polished at a high polishing rate while keeping the etching rate low.
- the surface roughness (RMS) can be reduced and the layer has a flat surface (substrate). Can be obtained.
- a metal-containing layer (polishing object) can be polished to a smooth surface at a high polishing rate while keeping the etching rate low without increasing the abrasive concentration.
- the polishing object according to the present invention is a layer containing a metal.
- the layer containing a metal should just be a thing in which the surface used as grinding
- the metal-containing layer is a substrate made of metal, a layer containing a metal, or a substrate having a layer made of metal (eg, from a layer containing metal or a metal on a polymer or other metal substrate). It may be a substrate on which a layer to be formed is disposed.
- the layer containing a metal is a layer made of metal (for example, a substrate) or an object to be polished (for example, a substrate) having a layer made of a metal.
- the metal is not particularly limited.
- tungsten, copper, aluminum, cobalt, hafnium, nickel, titanium, tantalum, gold, silver, platinum, palladium, rhodium, ruthenium, iridium, osmium, and the like can be given.
- the metal may be contained in the form of an alloy or a metal compound. These metals may be used alone or in combination of two or more.
- the polishing composition of the present invention can be suitably used for a high integration technique brought about by miniaturization of an LSI manufacturing process, and is particularly suitable for polishing a material for plugs and via holes around a transistor.
- the metal is tungsten (that is, the polishing composition of the present invention is preferably used for polishing a polishing object having a layer containing tungsten).
- the polishing composition of the present invention comprises abrasive grains, an oxidizing agent, a dispersion medium, and an anticorrosive agent having an acidic functional group and a basic functional group.
- the polishing composition of the present invention essentially contains abrasive grains.
- the abrasive grains contained in the polishing composition have an action of mechanically polishing the object to be polished, and improve the polishing rate of the object to be polished by the polishing composition.
- the abrasive that can be used in the present invention may be any of inorganic particles, organic particles, and organic-inorganic composite particles.
- the inorganic particles include particles made of metal oxides such as silica, alumina, ceria, titania, silicon nitride particles, silicon carbide particles, and boron nitride particles.
- Specific examples of the organic particles include polymethyl methacrylate (PMMA) particles.
- PMMA polymethyl methacrylate
- the abrasive grains may be used alone or in combination of two or more.
- the abrasive grains may be a commercially available product or a synthetic product.
- silica is preferable, and colloidal silica is particularly preferable.
- ⁇ Abrasive grains may be surface-modified. Since ordinary colloidal silica has a zeta potential value close to zero under acidic conditions, silica particles are not electrically repelled with each other under acidic conditions and are likely to agglomerate. In contrast, abrasive grains whose surfaces are modified so that the zeta potential has a relatively large negative value even under acidic conditions are strongly repelled from each other and dispersed well even under acidic conditions. As a result, the storage stability of the polishing composition can be improved. Such surface-modified abrasive grains can be obtained, for example, by mixing a metal such as aluminum, titanium or zirconium or an oxide thereof with the abrasive grains and doping the surface of the abrasive grains.
- a metal such as aluminum, titanium or zirconium or an oxide thereof
- organic acid-fixed silica is preferable, and organic acid-fixed colloidal silica is particularly preferable.
- the organic acid is immobilized on the surface of the colloidal silica contained in the polishing composition, for example, by chemically bonding a functional group of the organic acid to the surface of the colloidal silica. If the colloidal silica and the organic acid are simply allowed to coexist, the organic acid is not fixed to the colloidal silica.
- sulfonic acid which is a kind of organic acid, on colloidal silica, see, for example, “Sulphonic acid-functionalized silica through quantitative oxide of thiol groups”, Chem. Commun. 246-247 (2003).
- a silane coupling agent having a thiol group such as 3-mercaptopropyltrimethoxysilane is coupled to colloidal silica and then oxidized with hydrogen peroxide to fix the sulfonic acid on the surface.
- the colloidal silica thus obtained can be obtained.
- the carboxylic acid is immobilized on colloidal silica, for example, “Novel Silene Coupling Agents, Containing, Photo 28, 2-Nitrobenzyl Ester for GasotropyCarboxySportsGroxy 229 (2000).
- colloidal silica having a carboxylic acid immobilized on the surface can be obtained by irradiating light after coupling a silane coupling agent containing a photoreactive 2-nitrobenzyl ester to colloidal silica. .
- the average degree of association of the abrasive grains is also preferably less than 5.0, more preferably 3.0 or less, and even more preferably 2.5 or less. As the average degree of association of the abrasive grains decreases, the surface roughness due to the shape of the abrasive grains can be improved.
- the average degree of association of the abrasive grains is also preferably 1.0 or more, and more preferably 1.05 or more. As the average degree of association of the abrasive grains increases, there is an advantageous effect that the polishing rate of the object to be polished by the polishing composition is improved.
- the average degree of association is obtained by dividing the value of the average secondary particle diameter of the abrasive grains by the value of the average primary particle diameter.
- the lower limit of the average primary particle diameter of the abrasive grains is preferably 10 nm or more, more preferably 15 nm or more, and further preferably 20 nm or more.
- the upper limit of the average primary particle diameter of the abrasive grains is preferably 200 nm or less, more preferably 150 nm or less, and further preferably 100 nm or less.
- the polishing rate of the object to be polished by the polishing composition is improved, and the occurrence of surface defects on the surface of the object to be polished after polishing with the polishing composition is further suppressed. be able to.
- the average primary particle diameter of an abrasive grain is calculated based on the specific surface area of the abrasive grain measured by BET method, for example.
- the lower limit of the average secondary particle diameter of the abrasive grains is preferably 15 nm or more, more preferably 20 nm or more, and further preferably 30 nm or more.
- the upper limit of the average secondary particle diameter of the abrasive grains is preferably 300 nm or less, more preferably 260 nm or less, and further preferably 220 nm or less.
- the secondary particles referred to here are particles formed by association of abrasive grains in the polishing composition, and the average secondary particle diameter of the secondary particles is measured by, for example, a dynamic light scattering method. be able to.
- the upper limit of the aspect ratio of the abrasive grains in the polishing composition is less than 2.0, preferably 1.8 or less, and more preferably 1.5 or less. Within such a range, the surface roughness caused by the shape of the abrasive grains can be made favorable.
- the aspect ratio is a value obtained by taking the smallest rectangle circumscribing the image of the abrasive grains with a scanning electron microscope and dividing the length of the long side of the rectangle by the length of the short side of the same rectangle. And can be obtained using general image analysis software.
- the lower limit of the aspect ratio of the abrasive grains in the polishing composition is 1.0 or more. The closer to this value, the better the surface roughness due to the shape of the abrasive grains.
- the particle diameter (D90) and the total particle weight of all particles when the cumulative particle weight reaches 90% of the total particle weight from the fine particle side in the particle size distribution obtained by the laser diffraction scattering method in the abrasive grains in the polishing composition The lower limit of D90 / D10, which is the ratio to the particle diameter (D10) when reaching 10%, is 1.1 or more, preferably 1.2 or more, and preferably 1.3 or more. More preferred.
- the upper limit of the ratio D90 / D10 to the particle diameter (D10) when reaching 10% of the particle weight is not particularly limited, but is preferably 2.04 or less. Within such a range, the surface roughness caused by the shape of the abrasive grains can be made favorable.
- the lower limit of the content of the abrasive grains in the polishing composition is preferably 0.1% by mass or more, more preferably 0.5% by mass or more, and most preferably 1% by mass or more.
- the upper limit of the content of the abrasive grains in the polishing composition is preferably 50% by mass or less, more preferably 30% by mass or less, and further preferably 20% by mass or less. Within such a range, the polishing rate of the polishing object can be improved, and the cost of the polishing composition can be reduced, and the surface on the surface of the polishing object after polishing with the polishing composition can be reduced. It is possible to further suppress the occurrence of defects.
- the polishing composition of the present invention essentially contains an anticorrosive agent having an acidic functional group and a basic functional group. Due to the presence of the anticorrosive agent, dissolution (elution) of the metal contained in the object to be polished is suppressed, and the layer containing the metal (the object to be polished) can be polished smoothly (with low surface roughness (RMS)). Further, the metal-containing layer (polishing object) can be polished at a high polishing rate while keeping the etching rate low.
- an anticorrosive agent having an acidic functional group and a basic functional group. Due to the presence of the anticorrosive agent, dissolution (elution) of the metal contained in the object to be polished is suppressed, and the layer containing the metal (the object to be polished) can be polished smoothly (with low surface roughness (RMS)). Further, the metal-containing layer (polishing object) can be polished at a high polishing rate while keeping the etching rate low.
- the acidic functional group of the anticorrosive according to the present invention examples include a carboxyl group, an acid anhydride group, a sulfo group, a thiol group, a phosphoric acid group, an acidic phosphoric ester group, a phosphonic acid group, and a group of these salts.
- the acidic functional group of the anticorrosive agent is preferably a carboxyl group, a phosphate group, an acidic phosphate group, or a group of these salts.
- the acidic phosphate group is a group in which some phosphorus-bonded hydroxyl groups are alkoxylated.
- the alkoxy group include lower alkoxy groups such as a methoxy group, an ethoxy group, and a propoxy group.
- the number of carbon atoms of the lower alkoxy group is preferably 1-8.
- Examples of the basic functional group of the anticorrosive agent according to the present invention include an amino group, an imino group, an ammonium base, and a heterocyclic group having a basic nitrogen atom.
- the basic functional group of the anticorrosive agent is preferably an amino group or an ammonium base.
- the amino group may be a substituted or unsubstituted primary amino group, secondary amino group, or tertiary amino group.
- the ammonium base may be a tertiary ammonium base or a quaternary ammonium base.
- the acid value of the anticorrosive according to the present invention is preferably 5 to 300 mgKOH / g, more preferably 5 to 150 mgKOH / g.
- the amine value of the anticorrosive agent according to the present invention is preferably 5 to 300 mgKOH / g, and more preferably 5 to 150 mgKOH / g. That is, according to a preferred embodiment of the present invention, the acid value of the anticorrosive is 5 to 150 mgKOH / g and the amine value is 5 to 150 mgKOH / g.
- the anticorrosive agent can effectively form an anticorrosive film on the surface of the object to be polished without causing aggregation of abrasive grains.
- “acid value” represents the acid value per 1 g of the solid content of the anticorrosive agent according to the present invention, and can be determined by potentiometric titration according to JIS-K-0070.
- the “amine value” represents the amine value per 1 g of the solid content of the anticorrosive agent according to the present invention. The value is calculated by the potentiometric titration method using a 0.1N hydrochloric acid aqueous solution, and then converted into the equivalent value of potassium hydroxide. Say.
- Acidic functional groups adsorb on the surface of the metal oxide that is the object to be polished in a self-organized manner, and basic functional groups adsorb on the surface of the metal oxide that is the object to be polished having a negative zeta potential.
- the anticorrosive forms a film on the surface of the metal oxide.
- the anticorrosive agent having an acidic functional group and a basic functional group of the present invention is preferably a polymer anticorrosive agent.
- the weight average molecular weight of the anticorrosive is usually 1,000 or more.
- the weight average molecular weight is preferably 1,000 to 100,000, and more preferably 1,000 to 10,000. If the weight average molecular weight of the anticorrosive is 1,000 or more, the acidic or basic functional group of the anticorrosive adsorbs on the surface of the object to be polished, and effectively forms an anticorrosion film with the polymer chain portion of the anticorrosive. it can.
- the weight average molecular weight of the anticorrosive agent is 100,000 or less, aggregation with abrasive grains is prevented.
- the weight average molecular weight can be measured by gel permeation chromatography (GPC) using polystyrene as a standard substance.
- GPC gel permeation chromatography
- the binding position of the acidic functional group and the basic functional group to the polymer is not particularly limited and may be a main chain or a side chain. Both main chain and side chain may be used.
- the anticorrosive having an acidic functional group and a basic functional group is a compound represented by the following formula (1):
- R 1 and R 2 are each independently a hydrogen atom or a substituted or unsubstituted linear or branched alkyl group having 8 to 16 carbon atoms. Specific examples include a substituted or unsubstituted octyl group, nonyl group, decyl group, undecyl group, dodecyl group, tridecyl group, tetradecyl group, pentadecyl group, hexadecyl group, etc.
- n- Octyl group, n-decyl group, n-undecyl group, lauryl group (n-dodecyl group), n-tridecyl group, n-tetradecyl group, n-pentadecyl group, isotridecyl group, s-tridecyl group, t-tridecyl group can be mentioned.
- a substituted or unsubstituted linear or branched alkyl group having 12 to 15 carbon atoms is preferable from the viewpoint of suppressing the etching rate.
- a substituted or unsubstituted linear or branched alkyl group having 13 carbon atoms is more preferable.
- Y 1 and Y 2 are each independently a single bond or a group represented by the following formula (i), and at least one of Y 1 and Y 2 is a group represented by the following formula (i);
- R 3 is an alkylene group having 2 to 6 carbon atoms. Specific examples include an ethylene group, an n-propylene group, an i-propylene group, an n-butylene group, an i-butylene group, an n-pentylene group, and an n-hexylene group, and a plurality of R 3 are the same. Or different. Among these, R 3 is preferably an ethylene group from the viewpoint of more effectively exerting the effects of the present invention.
- N is an integer of 2 to 200, and among them, n is preferably an integer of 4 to 200, more preferably an integer of 4 to 130, from the viewpoint of suppressing the etching rate.
- X + is an ammonium ion, a primary ammonium ion, a secondary ammonium ion, a tertiary ammonium ion, or a quaternary ammonium ion. Specific examples include ammonium ion, methylammonium ion, dimethylammonium ion, trimethylethylammonium ion, trimethylpropylammonium ion, trimethylhexylammonium ion, tetrapentylammonium ion and the like. Among these, X + is an ammonium ion (NH 4 + ).
- the anticorrosive agent according to the present invention may be used alone or in combination of two or more.
- the anticorrosive agent according to the present invention may be a synthetic product or a commercially available product.
- a synthetic polymer When using a polymer anticorrosive as an anticorrosive having an acidic functional group and a basic functional group, a synthetic polymer may be used.
- synthetic polymers that can be used are vinyl polymerization polymers and condensation polymerization polymers.
- the acidic functional group and the basic functional group in the vinyl polymerization polymer having an acidic functional group and a basic functional group are derived from monomers at the time of vinyl polymerization, respectively.
- vinyl monomers having an acidic functional group include carboxyls such as acrylic acid, methacrylic acid, maleic acid, maleic anhydride, itaconic acid, citraconic acid, crotonic acid, fumaric acid, maleic acid monoalkyl ester, and fumaric acid monoalkyl ester.
- Examples of monomers having basic functions include N, N-dimethylaminoethyl (meth) acrylate, N-methylaminoethyl (meth) acrylate, N, N-diethylaminoethyl (meth) acrylate, and N, N-dimethylaminopropyl.
- Examples include aminoalkyl group-containing acrylates such as (meth) acrylate, Nt-butylaminoethyl (meth) acrylate, N, N-dimethylaminobutyl (meth) acrylate, and aminoalkyl group-containing methacrylates.
- N, N-dimethyl Examples include aminoalkyl group-containing acrylamides such as aminoethyl (meth) acrylamide and N, N-dimethylaminopropyl (meth) acrylamide, and aminoalkyl group-containing methacrylamide.
- (meth) acryl means “acryl or methacryl”. Block polymerization may be performed after polymerizing the acidic functional group-containing vinyl monomer and the basic functional group-containing vinyl monomer, respectively, or only one of them may be polymerized and then the other graft-polymerized. Good.
- Polycondensation polymers such as polyurethane, polyester, polyoxyalkylene, polyoxyalkylene / polyester copolymer, polyamide, phenol resin, urea resin, melamine resin, polycarbonate, epoxy resin, alkyd resin, polyalkyleneimine (polyethyleneimine, etc.), Nitrogen-containing polymers such as polyvinyl pyrrolidone, polyallylamine, polyether polyamine (polyoxyethylene polyamine, etc.) are mentioned.
- the lower limit of the content of the anticorrosive agent in the polishing composition is preferably 0.001% by mass or more, more preferably 0.003% by mass or more, and 0.005% by mass or more. Is more preferable.
- the upper limit of the content of the anticorrosive agent in the polishing composition is preferably 1% by mass or less, more preferably 0.1% by mass or less, and 0.05% by mass or less. Is more preferable. If it is in such a range, the grinding
- the polishing composition of the present invention essentially contains an oxidizing agent.
- the oxidizing agent according to the present invention is not particularly limited, but a peroxide is preferable. That is, according to a preferred embodiment of the present invention, the oxidizing agent is a peroxide. Specific examples of such peroxides include, but are not limited to, hydrogen peroxide, peracetic acid, percarbonate, urea peroxide, sodium persulfate, potassium persulfate, ammonium persulfate, potassium monopersulfate and oxone. Etc.
- the oxidizing agents may be used alone or in combination of two or more.
- the peroxide is a group consisting of hydrogen peroxide, peracetic acid, percarbonate, urea peroxide, sodium persulfate, potassium persulfate, ammonium persulfate, potassium monopersulfate and oxone. It is at least one selected from more.
- persulfates sodium persulfate, potassium persulfate, ammonium persulfate
- hydrogen peroxide is particularly preferable.
- the lower limit of the content (concentration) of the oxidizing agent in the polishing composition is preferably 0.001% by mass or more, more preferably 0.005% by mass or more, and 0.01% by mass or more. More preferably it is. There is an advantage that the polishing rate by the polishing composition is improved as the content of the oxidizing agent is increased. Further, the upper limit of the content (concentration) of the oxidizing agent in the polishing composition is preferably 10% by mass or less, more preferably 5% by mass or less, and further preferably 1% by mass or less. preferable.
- the material cost of the polishing composition can be reduced, and the processing of the polishing composition after polishing, that is, the advantage of reducing the load of waste liquid treatment can be achieved.
- the processing of the polishing composition after polishing that is, the advantage of reducing the load of waste liquid treatment can be achieved.
- excessive oxidation of the surface of the object to be polished is less likely to occur, and there is an advantage of reducing the roughness of the metal surface after polishing.
- an oxide film is formed on the surface of the layer containing a metal by an oxidizing agent, it is preferable to add the oxidizing agent immediately before polishing.
- the polishing composition of the present invention contains a dispersion medium in order to disperse or dissolve each component.
- the dispersion medium is not particularly limited, but water is preferable. From the viewpoint of suppressing the inhibition of the action of other components, water containing as little impurities as possible is more preferable. Specifically, after removing impurity ions with an ion exchange resin, foreign matters are removed through a filter. Pure water, ultrapure water, or distilled water is preferred.
- the polishing composition of the present invention essentially contains abrasive grains, an oxidizing agent, an anticorrosive agent, and a dispersion medium, but may contain other additives in addition to the above components.
- the additive normally added to polishing composition can be used. Specific examples include a pH adjuster, a complexing agent, a metal anticorrosive, an antiseptic, an antifungal agent, a reducing agent, a water-soluble polymer, an organic solvent for dissolving a hardly soluble organic substance, and the like.
- the polishing composition of the present invention does not substantially contain a diquaternary compound described in, for example, JP2013-42131A.
- the polishing composition of the present invention does not substantially contain an iodine compound (for example, potassium iodate) that can trigger generation of iodine gas.
- substantially free means that the target substance is present in a proportion of 10% by mass or less (lower limit: 0% by mass) with respect to the polishing composition. % Or less (lower limit: 0% by mass).
- the polishing composition of the present invention may further contain a pH adjuster.
- the pH can be adjusted by adding an appropriate amount of a pH adjusting agent.
- the pH adjuster used as necessary to adjust the pH of the polishing composition to a desired value may be either acid or alkali, and may be either an inorganic compound or an organic compound. Good.
- the acid include, for example, inorganic acids such as sulfuric acid, nitric acid, boric acid, carbonic acid, hypophosphorous acid, phosphorous acid and phosphoric acid; formic acid, acetic acid, propionic acid, butyric acid, valeric acid, 2-methylbutyric acid , N-hexanoic acid, 3,3-dimethylbutyric acid, 2-ethylbutyric acid, 4-methylpentanoic acid, n-heptanoic acid, 2-methylhexanoic acid, n-octanoic acid, 2-ethylhexanoic acid, benzoic acid, glycol Acids, salicylic acid, glyceric acid, oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, maleic acid, phthalic acid, malic acid, tartaric acid, citric acid and lactic acid and other carboxylic acids, and methanesulf
- alkali examples include ammonia, amines such as ethylenediamine and piperazine, and quaternary ammonium salts such as tetramethylammonium and tetraethylammonium.
- pH regulators can be used alone or in combination of two or more.
- the lower limit of the pH of the polishing composition of the present invention is preferably 1.0 or more, more preferably 1.05 or more, and particularly preferably 1.1 or more. As the pH of the polishing composition increases, the handling of the polishing composition becomes easier.
- the upper limit of the pH of the polishing composition is preferably 7 or less, more preferably 5 or less, and particularly preferably 4.0 or less. As the pH of the polishing composition decreases, the polishing rate of the metal that is the polishing object is improved.
- the complexing agent that can be included if necessary in the polishing composition has a function of chemically etching the surface of the polishing object, and more effectively improves the polishing rate of the polishing object by the polishing composition. It can be made.
- complexing agents examples include inorganic acids or salts thereof, organic acids or salts thereof, nitrile compounds, amino acids, and chelating agents. These complexing agents may be used alone or in admixture of two or more.
- the complexing agent may be a commercially available product or a synthetic product.
- a salt of the inorganic acid or the organic acid may be used.
- a salt of a weak acid and a strong base a salt of a strong acid and a weak base, or a salt of a weak acid and a weak base
- a pH buffering action can be expected.
- salts include, for example, potassium chloride, sodium sulfate, potassium nitrate, potassium carbonate, potassium tetrafluoroborate, potassium pyrophosphate, potassium oxalate, trisodium citrate, (+)-potassium tartrate, hexafluoro A potassium phosphate etc. are mentioned.
- nitrile compounds include acetonitrile, aminoacetonitrile, propionitrile, butyronitrile, isobutyronitrile, benzonitrile, glutaronitrile, methoxyacetonitrile, and the like.
- amino acids include glycine, ⁇ -alanine, ⁇ -alanine, N-methylglycine, N, N-dimethylglycine, 2-aminobutyric acid, norvaline, valine, leucine, norleucine, isoleucine, phenylalanine, proline, sarcosine, Ornithine, lysine, taurine, serine, threonine, homoserine, tyrosine, bicine, tricine, 3,5-diiodo-tyrosine, ⁇ - (3,4-dihydroxyphenyl) -alanine, thyroxine, 4-hydroxy-proline, cysteine, methionine , Ethionine, lanthionine, cystathionine, cystine, cysteic acid, aspartic acid, glutamic acid, S- (carboxymethyl) -cysteine, 4-aminobutyric acid, asparagine, glutamine,
- chelating agents include nitrilotriacetic acid, diethylenetriaminepentaacetic acid, ethylenediaminetetraacetic acid, N, N, N-trimethylenephosphonic acid, ethylenediamine-N, N, N ′, N′-tetramethylenesulfonic acid, transcyclohexane Diamine tetraacetic acid, 1,2-diaminopropanetetraacetic acid, glycol ether diamine tetraacetic acid, ethylenediamine orthohydroxyphenylacetic acid, ethylenediamine disuccinic acid (SS form), N- (2-carboxylateethyl) -L-aspartic acid, ⁇ -Alanine diacetate, 2-phosphonobutane-1,2,4-tricarboxylic acid, 1-hydroxyethylidene-1,1-diphosphonic acid, N, N'-bis (2-hydroxybenzyl) ethylenediamine-N, N'-diace
- At least one selected from the group consisting of an inorganic acid or a salt thereof, a carboxylic acid or a salt thereof, and a nitrile compound is preferable, from the viewpoint of stability of a complex structure with a metal compound contained in a polishing object.
- An inorganic acid or a salt thereof is more preferable.
- the content (concentration) of the complexing agent is not particularly limited.
- the lower limit of the content (concentration) of the complexing agent is not particularly limited because the effect is exhibited even in a small amount, but is preferably 0.001 g / L or more, and 0.01 g / L or more. More preferably, it is more preferably 1 g / L or more.
- the upper limit of the content (concentration) of the complexing agent is preferably 20 g / L or less, more preferably 15 g / L or less, and further preferably 10 g / L or less. If it is such a range, the grinding
- the metal anticorrosive agent that can be included in the polishing composition if necessary is a metal anticorrosive agent other than the above-mentioned anticorrosive agents having an acidic functional group and a basic functional group. It acts to suppress deterioration of the surface condition such as surface roughness.
- the anticorrosive agent according to the present invention acts as a metal anticorrosive agent, the polishing composition of the present invention can sufficiently suppress and prevent the dissolution of metal without adding a metal anticorrosive agent separately.
- the metal anticorrosive that can be used is not particularly limited, but is preferably a heterocyclic compound or a surfactant.
- the number of heterocyclic rings in the heterocyclic compound is not particularly limited.
- the heterocyclic compound may be a monocyclic compound or a polycyclic compound having a condensed ring.
- These metal anticorrosives may be used alone or in combination of two or more.
- a commercially available product or a synthetic product may be used as the metal anticorrosive.
- isoindole compound indazole compound, purine compound, quinolidine compound, quinoline compound, isoquinoline compound, naphthyridine compound, phthalazine compound, quinoxaline compound, quinazoline compound, cinnoline compound, buteridine compound, thiazole compound, isothiazole compound, oxazole compound, iso Examples thereof include nitrogen-containing heterocyclic compounds such as oxazole compounds and furazane compounds.
- More specific examples include pyrazole compounds such as 1H-pyrazole, 4-nitro-3-pyrazolecarboxylic acid, 3,5-pyrazolecarboxylic acid, 3-amino-5-phenylpyrazole, 5 -Amino-3-phenylpyrazole, 3,4,5-tribromopyrazole, 3-aminopyrazole, 3,5-dimethylpyrazole, 3,5-dimethyl-1-hydroxymethylpyrazole, 3-methylpyrazole, 1-methyl Pyrazole, 3-amino-5-methylpyrazole, 4-amino-pyrazolo [3,4-d] pyrimidine, allopurinol, 4-chloro-1H-pyrazolo [3,4-D] pyrimidine, 3,4-dihydroxy-6 -Methylpyrazolo (3,4-B) -pyridine, 6-methyl-1H-pyrazolo [3,4-b] pyridine 3-amine, and the like.
- pyrazole compounds such as 1H-pyrazole, 4-
- imidazole compounds include imidazole, 1-methylimidazole, 2-methylimidazole, 4-methylimidazole, 1,2-dimethylpyrazole, 2-ethyl-4-methylimidazole, 2-isopropylimidazole, benzimidazole, 5,6-dimethylbenzimidazole, 2-aminobenzimidazole, 2-chlorobenzimidazole, 2-methylbenzimidazole, 2- (1-hydroxyethyl) benzimidazole, 2-hydroxybenzimidazole, 2-phenylbenzimidazole, 2 , 5-dimethylbenzimidazole, 5-methylbenzimidazole, 5-nitrobenzimidazole and the like.
- triazole compounds include, for example, 1,2,3-triazole (1H-BTA), 1,2,4-triazole, 1-methyl-1,2,4-triazole, methyl-1H-1,2, 4-triazole-3-carboxylate, 1,2,4-triazole-3-carboxylic acid, methyl 1,2,4-triazole-3-carboxylate, 1H-1,2,4-triazole-3-thiol, 3,5-diamino-1H-1,2,4-triazole, 3-amino-1,2,4-triazole-5-thiol, 3-amino-1H-1,2,4-triazole, 3-amino- 5-benzyl-4H-1,2,4-triazole, 3-amino-5-methyl-4H-1,2,4-triazole, 3-nitro-1,2,4-triazole, 3-bromo-5 Nitro 1,2,4-triazole, 4- (1,2,4-triazol-1-yl) phenol, 4-amino-1,2,4-triazole, 4-amino
- tetrazole compounds include 1H-tetrazole, 5-methyltetrazole, 5-aminotetrazole, 5-phenyltetrazole, and the like.
- indazole compounds include, for example, 1H-indazole, 5-amino-1H-indazole, 5-nitro-1H-indazole, 5-hydroxy-1H-indazole, 6-amino-1H-indazole, 6-nitro-1H -Indazole, 6-hydroxy-1H-indazole, 3-carboxy-5-methyl-1H-indazole and the like.
- indole compounds include, for example, 1H-indole, 1-methyl-1H-indole, 2-methyl-1H-indole, 3-methyl-1H-indole, 4-methyl-1H-indole, 5-methyl-1H- Indole, 6-methyl-1H-indole, 7-methyl-1H-indole, 4-amino-1H-indole, 5-amino-1H-indole, 6-amino-1H-indole, 7-amino-1H-indole, 4-hydroxy-1H-indole, 5-hydroxy-1H-indole, 6-hydroxy-1H-indole, 7-hydroxy-1H-indole, 4-methoxy-1H-indole, 5-methoxy-1H-indole, 6- Methoxy-1H-indole, 7-methoxy-1H-indole, 4-chloro-1H Indole, 5-chloro-1H-indole, 6-chloro-1H Indo
- heterocyclic compounds are triazole compounds, and in particular, 1H-benzotriazole, 5-methyl-1H-benzotriazole, 5,6-dimethyl-1H-benzotriazole, 1- [N, N-bis (hydroxy Ethyl) aminomethyl] -5-methylbenzotriazole, 1- [N, N-bis (hydroxyethyl) aminomethyl] -4-methylbenzotriazole, 1,2,3-triazole, and 1,2,4-triazole Is preferred. Since these heterocyclic compounds have high chemical or physical adsorptive power to the surface of the object to be polished, a stronger protective film can be formed on the surface of the object to be polished. This is advantageous in improving the smoothness of the surface of the object to be polished after polishing with the polishing composition of the present invention.
- examples of the surfactant used as a metal anticorrosive include an anionic surfactant, a cationic surfactant, and an amphoteric surfactant.
- anionic surfactants include, for example, polyoxyethylene alkyl ether acetic acid, polyoxyethylene alkyl sulfuric acid ester, alkyl sulfuric acid ester, polyoxyethylene alkyl ether sulfuric acid, alkyl ether sulfuric acid, alkylbenzene sulfonic acid, alkyl phosphoric acid ester , Polyoxyethylene alkyl phosphate ester, polyoxyethylene sulfosuccinic acid, alkyl sulfosuccinic acid, alkyl naphthalene sulfonic acid, alkyl diphenyl ether disulfonic acid, and salts thereof.
- Examples of the cationic surfactant include alkyl trimethyl ammonium salt, alkyl dimethyl ammonium salt, alkyl benzyl dimethyl ammonium salt, alkyl amine salt and the like.
- amphoteric surfactants include alkyl betaines and alkyl amine oxides.
- nonionic surfactants include, for example, polyoxyalkylene alkyl ethers such as polyoxyethylene alkyl ether, sorbitan fatty acid esters, glycerin fatty acid esters, polyoxyethylene fatty acid esters, polyoxyethylene alkyl amines, and alkyl alkanols. Amides are mentioned. Of these, polyoxyalkylene alkyl ether is preferred.
- preferable surfactants are polyoxyethylene alkyl ether acetic acid, polyoxyethylene alkyl ether sulfate, alkyl ether sulfate, and alkylbenzene sulfonate. Since these surfactants have a high chemical or physical adsorption force to the surface of the object to be polished, a stronger protective film can be formed on the surface of the object to be polished. This is advantageous in improving the flatness of the surface of the object to be polished after polishing using the polishing composition of the present invention.
- the content (concentration) of the metal anticorrosive when the polishing composition contains the metal anticorrosive is not particularly limited.
- the lower limit of the content (concentration) of the metal anticorrosive is preferably 0.001 g / L or more, more preferably 0.005 g / L or more, and 0.01 g / L or more.
- the upper limit of the content (concentration) of the metal anticorrosive is preferably 10 g / L or less, more preferably 5 g / L or less, and further preferably 2 g / L or less. If it is such a range, melt
- antiseptics and fungicides that may be included in the polishing composition if necessary include, for example, 2-methyl-4-isothiazolin-3-one and 5-chloro-2-methyl-4-isothiazoline-3 -Isothiazoline preservatives such as ON, paraoxybenzoates, phenoxyethanol and the like. These antiseptics and fungicides may be used alone or in combination of two or more.
- the production method of the polishing composition of the present invention is not particularly limited, and for example, abrasive grains, an oxidizing agent, an anticorrosive agent, and other additives as necessary are stirred and mixed in a dispersion medium (for example, water). Can be obtained.
- the oxidant promotes the formation of an oxide film on the surface of the metal-containing layer, so that abrasive grains, anticorrosives and other additives as necessary are added to the dispersion medium (for example, water).
- a method for producing a polishing composition comprising a step of preparing a preliminary composition and a step of adding an oxidizing agent to the preliminary composition immediately before polishing is preferable.
- a polishing composition comprising a step of preparing a preliminary composition by mixing abrasive grains and an anticorrosive agent with a dispersion medium, and a step of adding an oxidizing agent to the preliminary composition immediately before polishing.
- the temperature at the time of mixing each component is not particularly limited, but is preferably 10 to 40 ° C., and may be heated to increase the dissolution rate. Further, the mixing time is not particularly limited as long as uniform mixing can be performed.
- the polishing composition of the present invention is suitably used for polishing a metal-containing layer (polishing object). Therefore, this invention also provides the grinding
- the metal in the polishing method and the substrate manufacturing method is preferably tungsten.
- a polishing apparatus As a polishing apparatus, a general holder having a polishing surface plate on which a holder for holding a substrate having a polishing object and a motor capable of changing the number of rotations are attached and a polishing pad (polishing cloth) can be attached.
- a polishing apparatus can be used.
- polishing pad a general nonwoven fabric, polyurethane, porous fluororesin, or the like can be used without particular limitation. It is preferable that the polishing pad is grooved so that the polishing liquid accumulates.
- the rotational speed of the polishing platen is preferably 10 to 500 rpm.
- the pressure applied to the substrate having the object to be polished is preferably 0.5 to 10 psi.
- the method of supplying the polishing composition to the polishing pad is not particularly limited, and for example, a method of continuously supplying with a pump or the like is employed. Although the supply amount is not limited, it is preferable that the surface of the polishing pad is always covered with the polishing composition of the present invention.
- the substrate After completion of polishing, the substrate is washed in running water, and water droplets adhering to the substrate are removed by a spin dryer or the like, and dried to obtain a substrate having a metal-containing layer.
- the polishing composition of the present invention may be a one-component type or a multi-component type including a two-component type.
- the oxidizing agent promotes the formation of an oxide film on the surface of the layer containing a metal.
- a two-component type consisting of a liquid is preferred.
- the polishing composition of the present invention may be prepared by diluting the stock solution of the polishing composition, for example, 10 times or more using a diluent such as water.
- the polishing composition of the present invention is preferably used in a metal polishing step, particularly a tungsten polishing step. Further, the polishing composition of the present invention comprises a tungsten polishing step, a main polishing step performed to remove most of the tungsten-containing layer, and a buff polishing step for final polishing the tungsten-containing layer and the insulator layer. It is preferably used in the buffing process when roughly classified into
- Example> In 1 L of pure water, the anticorrosive agent shown in Table 1 below is 0.01% by mass with respect to the final polishing composition, abrasive grains (sulfonic acid-fixed colloidal silica; average primary particle size: 30 nm, average secondary particle size) : 60 nm, aspect ratio: 1.24, D90 / D10: 2.01) is added in an amount of 2.0 mass% with respect to the final polishing composition, and the polishing composition has a pH of 2.1. Each preliminary composition was prepared by adding an aqueous maleic acid solution (30% by mass).
- each polishing composition was prepared.
- the pH of the composition liquid temperature: 25 ° C.
- polishing rate Removal Rate
- etching rate Etching Rate
- surface roughness RMS
- polishing object is polished under the following polishing conditions.
- the thickness (film thickness) of the object to be polished before and after polishing was measured with a manual sheet resistor (VR-120, manufactured by Hitachi Kokusai Electric Co., Ltd.).
- the polishing rate (removal rate) ( ⁇ / min) was determined by dividing the difference in thickness (film thickness) of the polishing object before and after polishing by the polishing time, as described in the following polishing rate calculation method.
- a tungsten wafer size: 32 mm ⁇ 32 mm was used as an object to be polished.
- Polishing machine Single-side CMP polishing machine (ENGIS) Polishing pad: Polyurethane pad (IC1010: manufactured by Rohm and Haas) Pressure: 2.0 psi Platen (surface plate) rotation speed: 70 rpm Head (carrier) rotation speed: 70 rpm Flow rate of polishing composition: 150 ml / min Polishing time: 60 sec (Calculation method of polishing rate) The polishing rate (polishing rate) ( ⁇ / min) is calculated by the following formula (1).
- etching test was performed by the following operation. That is, the polishing object was immersed for 10 minutes while putting 300 mL of each polishing composition in a sample container and stirring at 300 rpm. The wafer after immersion was washed with pure water for 30 seconds and dried by air blow drying with an air gun. The thickness (film thickness) of the object to be polished before and after the etching test was measured with a manual sheet resistor (VR-120, Hitachi Kokusai Electric). The etching rate ( ⁇ / min) was determined by dividing the difference in thickness (film thickness) of the object to be polished before and after the etching test by the etching test time as described in the following etching rate calculation method. A tungsten wafer (size: 32 mm ⁇ 32 mm) was used as an object to be polished.
- etching rate calculation method The etching rate (etching rate) ( ⁇ / min) is calculated by the following formula (2).
- RMS surface roughness
- POE polyoxyethylene
- number after POE means the number of moles of ethylene oxide added.
- POE (130) isotridecyl ether ammonium phosphate refers to a compound with 130 moles of ethylene oxide added.
- C12-15 means alkyl groups having 12 to 15 carbon atoms and mixtures thereof.
- a substrate having a polished surface with a smaller surface roughness (RMS) ie, excellent smoothness
- RMS surface roughness
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Abstract
L'invention concerne une composition de polissage qui est utilisée pour le polissage d'un objet de polissage ayant une couche qui contient un métal et qui permet d'obtenir une planarisation suffisante. À cet effet, l'invention porte sur une composition de polissage qui est utilisée pour le polissage d'un objet de polissage ayant une couche qui contient un métal et qui contient des grains abrasifs, un oxydant, un milieu de dispersion et un agent anticorrosion qui a un groupe fonctionnel acide et un groupe fonctionnel basique.
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