WO2016158648A1 - 化学機械研磨用処理組成物、化学機械研磨方法および洗浄方法 - Google Patents
化学機械研磨用処理組成物、化学機械研磨方法および洗浄方法 Download PDFInfo
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- WO2016158648A1 WO2016158648A1 PCT/JP2016/059324 JP2016059324W WO2016158648A1 WO 2016158648 A1 WO2016158648 A1 WO 2016158648A1 JP 2016059324 W JP2016059324 W JP 2016059324W WO 2016158648 A1 WO2016158648 A1 WO 2016158648A1
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- chemical mechanical
- mechanical polishing
- treatment composition
- polishing treatment
- cleaning
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- 238000005268 plasma chemical vapour deposition Methods 0.000 description 1
- 229920000052 poly(p-xylylene) Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 1
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 1
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 1
- 235000010483 polyoxyethylene sorbitan monopalmitate Nutrition 0.000 description 1
- 239000000249 polyoxyethylene sorbitan monopalmitate Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 229940035044 sorbitan monolaurate Drugs 0.000 description 1
- 235000011071 sorbitan monopalmitate Nutrition 0.000 description 1
- 239000001570 sorbitan monopalmitate Substances 0.000 description 1
- 229940031953 sorbitan monopalmitate Drugs 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 239000010421 standard material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000003440 styrenes Chemical class 0.000 description 1
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 1
- 238000002230 thermal chemical vapour deposition Methods 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000004506 ultrasonic cleaning 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
- C09G1/04—Aqueous dispersions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/11—Lapping tools
- B24B37/20—Lapping pads for working plane surfaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B57/00—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents
- B24B57/02—Devices for feeding, applying, grading or recovering grinding, polishing or lapping agents for feeding of fluid, sprayed, pulverised, or liquefied grinding, polishing or lapping agents
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/14—Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
- C23G1/20—Other heavy metals
-
- 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
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/02068—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers
- H01L21/02074—Cleaning during device manufacture during, before or after processing of conductive layers, e.g. polysilicon or amorphous silicon layers the processing being a planarization of conductive layers
-
- 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
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
-
- 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
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/32115—Planarisation
- H01L21/3212—Planarisation by chemical mechanical polishing [CMP]
-
- 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
- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
- H01L21/4814—Conductive parts
- H01L21/4846—Leads on or in insulating or insulated substrates, e.g. metallisation
-
- 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
- H01L21/48—Manufacture or treatment of parts, e.g. containers, prior to assembly of the devices, using processes not provided for in a single one of the subgroups H01L21/06 - H01L21/326
- H01L21/4814—Conductive parts
- H01L21/4846—Leads on or in insulating or insulated substrates, e.g. metallisation
- H01L21/4864—Cleaning, e.g. removing of solder
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L23/00—Details of semiconductor or other solid state devices
- H01L23/48—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor
- H01L23/488—Arrangements for conducting electric current to or from the solid state body in operation, e.g. leads, terminal arrangements ; Selection of materials therefor consisting of soldered or bonded constructions
- H01L23/498—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers
- H01L23/49866—Leads, i.e. metallisations or lead-frames on insulating substrates, e.g. chip carriers characterised by the materials
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/07—Treatments involving liquids, e.g. plating, rinsing
- H05K2203/0779—Treatments involving liquids, e.g. plating, rinsing characterised by the specific liquids involved
- H05K2203/0786—Using an aqueous solution, e.g. for cleaning or during drilling of holes
- H05K2203/0793—Aqueous alkaline solution, e.g. for cleaning or etching
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/26—Cleaning or polishing of the conductive pattern
Definitions
- the present invention relates to a chemical mechanical polishing treatment composition, a chemical mechanical polishing method, and a cleaning method.
- CMP Chemical Mechanical Polishing
- the object is chemically bonded to the polishing pad by sliding the object and the polishing pad against each other while supplying the chemical mechanical polishing aqueous dispersion on the polishing pad.
- this is a mechanical polishing technique.
- a wiring substrate in a semiconductor device includes a wiring material and a barrier metal material for preventing diffusion of the wiring material into an inorganic material film. Copper and tungsten have been mainly used as wiring materials, and tantalum nitride and titanium nitride have been mainly used as barrier metal materials.
- the number of particles of 0.2 ⁇ m or more counts 10,000 or more, but it is required to remove several to tens of particles by cleaning.
- the surface concentration of metal impurities is 1 ⁇ 10 11 to 1 ⁇ 10 12 or more, but the customer is required to remove it to 1 ⁇ 10 10 or less by washing. .
- cleaning after CMP is an indispensable process that cannot be avoided.
- the conventional chemical mechanical polishing composition is insufficient in obtaining both a sufficient cobalt polishing rate and reducing cobalt corrosion.
- a surfactant or the like may be used to protect cobalt, but there is also a problem that the surfactant is adsorbed on the copper surface and a sufficient copper polishing rate is difficult to obtain.
- Chemical mechanical polishing treatment composition that can be flattened by chemical mechanical polishing and that can efficiently remove metal oxide films and organic residues on the wiring substrate, and polishing of the wiring substrate using the same A method and a cleaning method are provided.
- the present invention has been made to solve at least a part of the above-described problems, and can be realized as the following aspects or application examples.
- One aspect of the chemical mechanical polishing treatment composition for a wiring board according to the present invention is: (A) a water-soluble amine, (B) a water-soluble polymer having a repeating unit containing an aromatic hydrocarbon group, And an aqueous medium.
- the pH can be 9 or higher.
- the component (A) may be at least one selected from the group consisting of alkanolamine, hydroxylamine, morpholine, morpholine derivatives, piperazine, and piperazine derivatives.
- the component (B) can be a polymer having a structural unit derived from alkyl group-substituted or unsubstituted styrene.
- the component (C) can be at least one selected from the group consisting of phenylsuccinic acid, phenylalanine, benzoic acid, phenyllactic acid, and naphthalenesulfonic acid.
- the chemical mechanical polishing treatment composition is used for treating a surface to be treated of a wiring board
- the wiring board has a wiring material made of copper or tungsten and a barrier metal material made of at least one selected from the group consisting of tantalum, titanium, cobalt, ruthenium, manganese, and a compound thereof on a surface to be cleaned. Can be included.
- the surface to be cleaned can include a portion where the wiring material and the barrier metal material are in contact with each other.
- the chemical mechanical polishing treatment composition may be a cleaning composition for cleaning the surface to be treated.
- the chemical mechanical polishing composition may be a chemical mechanical polishing composition for polishing the surface to be processed.
- One aspect of the chemical mechanical polishing method according to the present invention is: Using the chemical mechanical polishing treatment composition described in Application Example 11 above, the surface to be treated is polished.
- One aspect of the cleaning method according to the present invention is: The treatment surface is cleaned using the chemical mechanical polishing treatment composition described in Application Example 9 above.
- the chemical mechanical polishing treatment composition of the present invention it is possible to simultaneously suppress the occurrence of corrosion and defects in the wiring material and the barrier metal material used in the wiring substrate, and to planarize the wiring layer by chemical mechanical polishing. it can. Moreover, the metal oxide film and organic residue on the wiring substrate can be efficiently removed.
- FIG. 1 is a cross-sectional view schematically showing an object to be processed for performing the chemical mechanical polishing method according to the present embodiment.
- FIG. 2 is a cross-sectional view schematically showing an object to be processed after the first polishing step.
- FIG. 3 is a cross-sectional view schematically showing an object to be processed after the second polishing step.
- a chemical mechanical polishing treatment composition according to an embodiment of the present invention includes (A) a water-soluble amine (hereinafter also referred to as “component (A)”), (B) an aromatic hydrocarbon.
- component (A) a water-soluble amine
- component (B) an aromatic hydrocarbon.
- component (B) a water-soluble polymer having a repeating unit containing a group
- component (B) an aqueous medium
- the chemical mechanical polishing treatment composition according to this embodiment can be used as a “chemical mechanical polishing composition” for polishing a surface to be processed.
- it preferably contains (D) abrasive grains (hereinafter also referred to as “component (D)”).
- component (D) abrasive grains
- the chemical mechanical polishing treatment composition according to the present embodiment for example, sputtering a conductive metal such as aluminum, copper, or tungsten into fine grooves or holes provided in an insulating film such as silicon oxide on a semiconductor substrate. Then, after depositing by a method such as plating, the excessively laminated metal film is removed by CMP, and it can be used in a damascene process in which metal is left only in a portion of a minute groove or hole.
- the chemical mechanical polishing treatment composition according to the present embodiment exhibits a particularly excellent effect when polishing is performed on a wiring substrate in which copper as a wiring material and cobalt and / or tantalum nitride as a barrier
- the chemical mechanical polishing treatment composition according to this embodiment can also be used as a “cleaning composition” for cleaning the surface to be treated.
- it can be used mainly as a cleaning agent for removing particles and metal impurities present on the surface of the wiring material and barrier metal material after the completion of CMP.
- the chemical mechanical polishing treatment composition according to the present embodiment as a cleaning composition, it is possible to simultaneously suppress the occurrence of corrosion and defects in the wiring material and the barrier metal material, Organic residues can be removed efficiently.
- the chemical mechanical polishing treatment composition according to the present embodiment is used as a cleaning composition, whereby a wiring substrate in which copper as a wiring material and cobalt and / or tantalum nitride as a barrier metal material coexist is treated. When it is performed, it exhibits a particularly excellent effect.
- the chemical mechanical polishing treatment composition according to this embodiment contains (A) a water-soluble amine.
- the inventor presumes that the component (A) has a function as a so-called etching agent.
- the chemical mechanical polishing treatment composition according to the present embodiment contains the component (A), so that a metal oxide film (for example, CuO, CuO, etc.) on the wiring substrate in the polishing step in CMP and the cleaning step after completion of CMP is contained.
- a metal oxide film for example, CuO, CuO, etc.
- organic residues eg, BTA layer
- water-soluble means that the mass dissolved in 100 g of water at 20 ° C. is 0.1 g or more.
- a alkanolamine, a primary amine, a secondary amine, a tertiary amine etc. are mentioned as a specific example.
- the alkanolamine is not particularly limited, but specific examples include monoethanolamine, diethanolamine, triethanolamine, N-methylethanolamine, N-methyl-N, N-diethanolamine, N, N-dimethylethanolamine, N, N-diethylethanolamine, N, N-dibutylethanolamine, N- ( ⁇ -aminoethyl) ethanolamine, N-ethylethanolamine, monopropanolamine, dipropanolamine, tripropanolamine, monoisopropanolamine, diisopropanolamine , Triisopropanolamine and the like.
- the primary amine is not particularly limited, but specific examples include methylamine, ethylamine, propylamine, butylamine, pentylamine, 1,3-propanediamine and the like. Although it does not specifically limit as a secondary amine, A piperidine, piperazine, etc. are mentioned as a specific example. Examples of the tertiary amine include trimethylamine and triethylamine. These (A) components may be used individually by 1 type, and may be used in mixture of 2 or more types.
- monoethanolamine and monoisopropanolamine are preferable, and monoethanolamine is more preferable in that the effect of etching the metal oxide film and organic residue on the wiring substrate is high.
- the content ratio of the component (A) is that of the chemical mechanical polishing composition.
- it is 0.0001 mass% or more and 1 mass% or less with respect to the total mass, More preferably, it is 0.0005 mass% or more and 0.5 mass% or less, Most preferably, it is 0.001 mass% or more and 0.1 mass% or less. It is.
- the content ratio of the component (A) is within the above range, it is possible to polish more effectively while reducing the corrosion of the metal on the wiring board without reducing the polishing rate in the wiring polishing step. .
- the content ratio of the component (A) is the cleaning composition. Is preferably 0.0001% by mass or more and 1% by mass or less, more preferably 0.0005% by mass or more and 0.5% by mass or less, and particularly preferably 0.001% by mass or more and 0.1% by mass. It is as follows. When the content ratio of the component (A) is in the above range, the metal oxide film and the organic residue on the wiring board are more effectively etched without corroding the surface to be cleaned in the cleaning process after the CMP is completed. Can be removed.
- the chemical mechanical polishing treatment composition according to this embodiment contains (B) a water-soluble polymer having a repeating unit containing an aromatic hydrocarbon group.
- the inventor presumes that the component (B) has a function of adsorbing to the surface of the surface to be polished to reduce corrosion. Therefore, it is considered that when the component (B) is added to the chemical mechanical polishing treatment composition, the corrosion of the surface to be treated can be reduced.
- the component (B) is not particularly limited as long as it has a repeating unit having an aromatic hydrocarbon group and is water-soluble.
- the polymer used in the component (B) is not particularly limited. Specific examples include monomers such as styrene, ⁇ -methylstyrene, 4-methylstyrene, and acid monomers such as (meth) acrylic acid and maleic acid. And a polymer obtained by condensing benzenesulfonic acid, naphthalenesulfonic acid and the like with formalin.
- These (B) components can be used individually by 1 type or in combination of 2 or more types.
- the weight average molecular weight (Mw) of the component (B) is preferably from 1,000 to 1,500,000, more preferably from 3,000 to 1,200,000.
- “weight average molecular weight” refers to a weight average molecular weight in terms of polyethylene glycol measured by GPC (gel permeation chromatography).
- the molecular weight analysis conditions are as follows. ⁇ Molecular weight measurement> The weight average molecular weight (Mw), number average molecular weight (Mn), and molecular weight distribution (Mw / Mn) of the polymer were measured by gel permeation chromatography under the following conditions. Column: “TSKgel ⁇ M” and “TSKgel ⁇ 2500” from Tosoh Corporation are connected in series. All column sizes are 7.8 x 300 mm. -Solvent: 0.1M sodium borate aqueous solution and acetonitrile were mixed at a ratio of 80:20 to make a total of 100.
- the content of the component (B) is preferably adjusted so that the chemical mechanical polishing treatment composition has a viscosity at room temperature of 2 mPa ⁇ s or less.
- the viscosity at room temperature of the chemical mechanical polishing treatment composition is 2 mPa ⁇ s or less, the chemical mechanical polishing treatment composition can be more effectively and stably supplied onto the polishing cloth. Further, since the viscosity is almost determined by the average molecular weight and content of the polymer, the viscosity may be adjusted in consideration of the balance.
- the content ratio of the component (B) is preferably 0 with respect to the total mass of the chemical mechanical polishing composition. It is 0.0001% by mass or more and 1% by mass or less, more preferably 0.0005% by mass or more and 0.1% by mass or less, and particularly preferably 0.001% by mass or more and 0.01% by mass or less.
- the content ratio of the component (B) is in the previous range, the surface to be processed can be more effectively polished while reducing the corrosion of the surface to be processed without decreasing the polishing rate.
- the content of the component (B) is preferably 0.0001% by mass with respect to the total mass of the cleaning composition.
- the content is 1% by mass or less, more preferably 0.0005% by mass or more and 0.1% by mass or less, and particularly preferably 0.001% by mass or more and 0.01% by mass or less.
- component (B) is physically adsorbed on the surface to be treated.
- the surface to be processed such as copper is processed using the chemical mechanical polishing treatment composition according to the present embodiment
- the surface to be processed is corroded more than necessary by the amine compound as an etching agent. It is thought to suppress this.
- the chemical mechanical polishing treatment composition according to this embodiment can contain (C) an organic acid having an aromatic hydrocarbon group (hereinafter also referred to as “C component”).
- Component (C) is a compound having one or more acidic groups such as a carboxy group and a sulfo group, and an aromatic hydrocarbon group in addition to the acidic group.
- the polymer is not included in the component (C).
- the corrosion potential of the wiring material and the barrier metal material on the wiring substrate can be controlled, and the difference in corrosion potential between the wiring material and the barrier metal material can be reduced. Thereby, it is considered that corrosion of each metal due to galvanic corrosion occurring between different metals can be suppressed.
- galvanic corrosion is a form of corrosion caused by contact of dissimilar metals, and generally when a metal having a different potential is brought into contact in an electrolytic solution such as water, a lower potential metal.
- an electrolytic solution such as water
- a lower potential metal Refers to the phenomenon of corrosion.
- the difference in corrosion potential between the wiring material and the barrier metal material can be reduced by adding the component (C). Thereby, it becomes possible to suppress corrosion of each metal due to galvanic corrosion that occurs between different metals.
- (C) Component is not particularly limited, but specific examples include benzoic acid, phenyl lactic acid, phenyl succinic acid, phenylalanine, naphthalene sulfonic acid and the like. These (C) components may be used alone or in combination of two or more.
- the content ratio of the component (C) is preferably 0 with respect to the total mass of the chemical mechanical polishing composition. It is 0.0001% by mass or more and 1% by mass or less, more preferably 0.0005% by mass or more and 0.5% by mass or less, and particularly preferably 0.001% by mass or more and 0.1% by mass or less.
- the content ratio of the component (C) is in the above range, the surface to be processed can be polished while reducing the corrosion of the surface to be processed without reducing the polishing rate. Further, the difference in corrosion potential between the wiring material on the wiring board and the barrier metal material can be reduced, and thereby galvanic corrosion of the wiring material and the barrier metal material can be more effectively suppressed.
- the content of the component (C) is preferably 0.0001% by mass with respect to the total mass of the cleaning composition.
- the content is 1% by mass or less, more preferably 0.0005% by mass or more and 0.5% by mass or less, and particularly preferably 0.001% by mass or more and 0.1% by mass or less.
- the silica particles are not particularly limited, but specific examples include colloidal silica and fumed silica. Among these, colloidal silica is preferable. Colloidal silica is preferably used from the viewpoint of reducing polishing defects such as scratches, and for example, those produced by the method described in JP-A-2003-109921 can be used. Also, JP 2010-269985A, J. Org. Ind. Eng. Chem. , Vol. 12, no. 6, (2006) 911-917 and the like, surface-modified colloidal silica may be used.
- the content ratio of the abrasive grains is 0.1% by mass or more and 10% by mass or less, preferably 0.1% by mass or more and 8% by mass or less, more preferably with respect to the total mass of the chemical mechanical polishing treatment composition. Is 0.1 mass% or more and 7 mass% or less.
- D When the content ratio of the abrasive grains is within the above range, a practical polishing rate for the tungsten film can be obtained.
- the chemical mechanical polishing treatment composition according to this embodiment preferably has a pH of 9 or more, more preferably 10 or more and 14 or less, and more preferably 10.5 or more and 13.5 or less. Further preferred.
- a protective surface such as the component (B) and the component (C) and an etching agent are likely to function on the surface of the wiring board, so that a good surface to be processed can be easily obtained. Become.
- the pH adjuster includes sodium hydroxide, potassium hydroxide, rubidium hydroxide, hydroxide It is preferable to use an alkali metal hydroxide such as cesium, an organic ammonium salt such as tetramethylammonium hydroxide, or a basic compound such as ammonia. These pH adjusting agents may be used alone or in combination of two or more.
- an alkali metal hydroxide such as sodium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide, etc. among these pH adjusters because of less health damage to the human body. Potassium oxide is more preferred.
- the chemical mechanical polishing treatment composition according to this embodiment contains an aqueous medium.
- the aqueous medium is not particularly limited as long as it can serve as a solvent mainly composed of water. As such an aqueous medium, it is more preferable to use water.
- a nonionic surfactant may be further added to the chemical mechanical polishing treatment composition according to this embodiment.
- the surfactant has an effect of imparting an appropriate viscosity to the chemical mechanical polishing treatment composition.
- the viscosity of the chemical mechanical polishing treatment composition is preferably adjusted to be 0.5 mPa ⁇ s or more and 2 mPa ⁇ s or less at 25 ° C.
- particles and metal impurities contained in the CMP slurry can be removed by adding a nonionic surfactant. The effect of removing from the wiring board is enhanced, and a better surface to be processed may be obtained.
- nonionic surfactants include polyoxyethylene alkyl ethers such as polyoxyethylene lauryl ether, polyoxyethylene cetyl ether, polyoxyethylene stearyl ether, polyoxyethylene oleyl ether; polyoxyethylene octylphenyl ether, polyoxy Polyoxyethylene aryl ethers such as ethylene nonylphenyl ether; sorbitan fatty acid esters such as sorbitan monolaurate, sorbitan monopalmitate, sorbitan monostearate; polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan monopalmitate, polyoxy And polyoxyethylene sorbitan fatty acid esters such as ethylene sorbitan monostearate.
- the nonionic surfactants exemplified above may be used singly or in combination of two or more.
- the content of the nonionic surfactant is preferably 0.001% by mass or more and 0% by mass. 0.1 mass% or less, more preferably 0.002 mass% or more and 0.05 mass% or less, particularly preferably 0.003 mass% or more and 0.03 mass% or less.
- the content ratio of the nonionic surfactant is in the previous range, it is possible to simultaneously suppress corrosion and defects of the wiring material and barrier metal material used for the wiring board and to flatten the wiring layer by chemical mechanical polishing. it can.
- the content of the nonionic surfactant is preferably 0.001% by mass or more and 1.0% with respect to the total mass. It is not more than mass%, more preferably not less than 0.002 mass% and not more than 0.1 mass%, particularly preferably not less than 0.003 mass% and not more than 0.05 mass%.
- the content ratio of the nonionic surfactant is in the previous range, the effect of removing particles and metal impurities contained in the CMP slurry from the wiring board is enhanced, and a better surface to be cleaned may be obtained. .
- the chemical mechanical polishing treatment composition according to the present embodiment is dramatically treated compared to the case where the component (B) and the component (C) are each used alone as a corrosion inhibitor. It is presumed that the surface corrosion inhibition effect is increased.
- the metal materials immersed in the chemical mechanical polishing treatment composition according to the present embodiment each exhibit a specific corrosion potential.
- the component (B) By interaction with the component (C), the absolute value of the corrosion potential difference between copper and cobalt can be made 0.1 V or less, and the absolute value of the corrosion potential difference between copper and tantalum nitride can be made 0.5 V or less. Therefore, the chemical mechanical polishing treatment composition according to the present embodiment is particularly effective in suppressing galvanic corrosion in a wiring board using copper as a wiring material and cobalt and / or tantalum nitride as a barrier metal material. be able to.
- the corrosion potential can be measured, for example, as follows. First, an electrochemical measurement device is prepared in which three electrodes, which are a working electrode (WE) of a test sample, a counter electrode (CE) for flowing current, and a reference electrode (RE) serving as a reference, are electrically connected to a potentiostat. To do. Next, the chemical mechanical polishing treatment composition according to this embodiment is placed in the cell, the three electrodes are immersed in the chemical mechanical polishing treatment composition in the cell, and a potential is applied by a potentiostat to measure the current. Thus, it can be obtained by measuring a potential-current curve.
- WE working electrode
- CE counter electrode
- RE reference electrode
- the chemical mechanical polishing composition according to the present embodiment can be suitably used as a chemical mechanical polishing composition when polishing a wiring board in CMP.
- the surface to be polished of the wiring substrate to be polished includes at least one selected from the group consisting of a wiring material made of copper, cobalt or tungsten and tantalum, titanium, cobalt, ruthenium, manganese, and a compound thereof. And a barrier metal material.
- the wiring material and the barrier metal material can be simultaneously corroded and the generation of defects can be suppressed, and the polishing can be performed without reducing the polishing rate.
- the chemical mechanical polishing treatment composition according to this embodiment can be suitably used as a wiring board cleaning agent when cleaning a wiring board after completion of CMP.
- the surface to be cleaned of the wiring board to be cleaned is made of at least one selected from the group consisting of a wiring material made of copper, cobalt or tungsten and tantalum, titanium, cobalt, ruthenium, manganese, and a compound thereof. And a barrier metal material.
- corrosion of the wiring material and barrier metal material and generation of defects can be suppressed at the same time, and oxide films and organic residues on the wiring board can be efficiently removed.
- the chemical mechanical polishing treatment composition according to this embodiment has an absolute value of the corrosion potential difference between copper and cobalt of 0.1 V or less and an absolute value of the corrosion potential difference between copper and tantalum nitride of 0.5 V or less. be able to. Therefore, galvanic corrosion is effective when using copper as a wiring material, cobalt and / or tantalum nitride as a barrier metal material, and polishing or cleaning a wiring board having a portion where the wiring material and the barrier metal material are in contact with each other. Can be suppressed.
- the method for preparing the chemical mechanical polishing treatment composition according to the present embodiment is not particularly limited.
- component (A), component (B), and (C) as necessary.
- Component, component (D), and nonionic surfactant are added to an aqueous medium and stirred and mixed to dissolve each component in the aqueous medium, and then a pH adjuster is added to adjust the pH to a predetermined value.
- a method is mentioned. There are no particular restrictions on the mixing order or mixing method of the components other than the pH adjuster.
- the chemical mechanical polishing treatment composition according to this embodiment can be used after diluting with an aqueous medium at the time of use.
- the chemical mechanical polishing or cleaning method according to this embodiment is characterized by including a step of chemical mechanical polishing or cleaning using the above-described chemical mechanical polishing processing composition.
- the chemical mechanical polishing or cleaning method according to this embodiment is not particularly limited, but one specific example will be described in detail below with reference to the drawings.
- a wiring substrate for performing the chemical mechanical polishing or cleaning method according to the present embodiment includes an insulating film having a recess, and a barrier metal film formed so as to cover a bottom surface or a side surface in the recess. And a metal oxide film embedded in the recess so as to cover the barrier metal film and serving as a wiring.
- the material of the barrier metal film includes at least one selected from the group consisting of tantalum, titanium, cobalt, ruthenium, manganese, and a compound thereof, and the metal oxide film embedded in the recess , Including copper or tungsten.
- this wiring board can be obtained by subjecting a workpiece to chemical mechanical polishing using a chemical mechanical polishing composition.
- FIG. 1 is a cross-sectional view schematically showing an object to be processed used for chemical mechanical polishing. First, the manufacturing method of the to-be-processed object 100 shown in FIG. 1 is demonstrated.
- the low dielectric constant insulating film 10 is formed by a coating method or a plasma CVD method.
- the low dielectric constant insulating film 10 include inorganic insulating films and organic insulating films.
- Parylene film (k 2.7 to 3.0)
- An insulating film 12 is formed on the low dielectric constant insulating film 10 by using a CVD method or a thermal oxidation method.
- the insulating film 12 is a film formed to protect the low dielectric constant insulating film 10 having low mechanical strength from polishing pressure or the like, and is also called a so-called cap layer.
- a silicon oxide film formed by a vacuum process for example, a PETEOS film (Plasma Enhanced-TEOS film), an HDP film (High Density Plasma Enhanced-TEOS film), or a thermal chemical vapor deposition method can be used.
- FSG Fluorine-doped silicate glass
- BPSG film boron phosphorous silicate film
- SiON Silicon oxynitride
- the wiring recess 11 is formed by etching the low dielectric constant insulating film 10 and the insulating film 12 so as to communicate with each other.
- the barrier metal film 14 is formed so as to cover the surface of the insulating film 12 and the bottom surface or side surface of the wiring recess 11 using the CVD method.
- the barrier metal film 14 include tantalum, titanium, cobalt, ruthenium, manganese, and compounds thereof.
- the barrier metal film 14 is often formed from one of these, but two or more kinds such as tantalum (Ta) and tantalum nitride (TaN) can be used in combination.
- the barrier metal film 14 is adhesive to the copper (or copper alloy) film and has a diffusion barrier property to the copper (or copper alloy) film. From the viewpoint of superiority, Ta or TaN is preferable.
- the object 100 is obtained by forming a metal oxide film 16 by depositing a metal on the barrier metal film 14 by a sputtering method or the like using a plating method.
- the metal for forming the metal oxide film 16 include copper (or copper alloy) and tungsten.
- polishing Step the chemical mechanical polishing is performed by pressing the object to be polished onto the polishing pad and sliding the object to be polished and the polishing pad against each other while supplying the chemical mechanical polishing composition onto the polishing pad. This is a technique for chemically and mechanically polishing an object to be polished.
- FIG. 2 is a cross-sectional view schematically showing the object to be processed after the first polishing step.
- FIG. 3 is a cross-sectional view schematically showing an object to be processed after the second polishing step.
- the unnecessary metal oxide film 16 deposited on the barrier metal film 14 of the object to be processed obtained in (1) is removed by CMP (first polishing step).
- CMP is performed using a predetermined chemical mechanical polishing aqueous dispersion, for example, a chemical mechanical polishing aqueous dispersion containing abrasive grains, carboxylic acid, an anionic surfactant, and the like.
- a predetermined chemical mechanical polishing aqueous dispersion for example, a chemical mechanical polishing aqueous dispersion containing abrasive grains, carboxylic acid, an anionic surfactant, and the like.
- the metal oxide film 16 is continuously polished until the barrier metal film 14 is exposed by CMP. After confirming that the barrier metal film 14 is exposed, the CMP is temporarily stopped.
- CMP second polishing step
- CMP is performed using a chemical mechanical polishing aqueous dispersion similar to or different from the first polishing step. As shown in FIG. 3, unnecessary films are continuously polished until the low dielectric constant insulating film 10 is exposed by CMP. In this way, the wiring substrate 200 having excellent flatness of the surface to be polished can be obtained.
- a commercially available chemical mechanical polishing apparatus can be used.
- a commercially available chemical mechanical polishing apparatus for example, “EPO-112”, “EPO-222” manufactured by Ebara Manufacturing Co., Ltd .; “LGP-510”, “LGP-552” manufactured by Lapmaster SFT, Applied Materials, Inc. Manufactured, model “Mirra” and the like.
- Preferred polishing conditions should be set as appropriate depending on the chemical mechanical polishing apparatus used. For example, when “EPO-112” is used as the chemical mechanical polishing apparatus, the following conditions may be used.
- Polishing pressure preferably 60 to 200 gf / cm 2 , more preferably 100 to 150 gf / cm 2
- Chemical chemical polishing treatment composition supply rate preferably 50 to 400 mL / min, more preferably 100 to 300 mL / min
- the surface (surface to be cleaned 200a) of the wiring substrate 200 shown in FIG. 3 is cleaned using the above-described cleaning composition.
- the surface to be cleaned 200a also includes a portion where the metal oxide film 16 that is a wiring material and the barrier metal film 14 formed of the barrier metal material are in contact with each other.
- the cleaning method is not particularly limited, but is performed by a method in which the above-described cleaning composition is brought into direct contact with the wiring substrate 200.
- a method of bringing the cleaning composition into direct contact with the wiring substrate 200 to-be-processed object 100 a dip type in which the cleaning composition is filled in the cleaning tank and the wiring substrate is immersed; the cleaning composition is allowed to flow down from the nozzle onto the wiring substrate.
- the method include a spin method in which the wiring substrate is rotated at a high speed, and a spray method in which the cleaning composition is sprayed on the wiring substrate for cleaning.
- a batch type cleaning apparatus that simultaneously cleans a plurality of wiring boards accommodated in a cassette, a single wafer cleaning that attaches and cleans one wiring board to a holder Examples thereof include an apparatus.
- the temperature of the cleaning composition is usually room temperature, but it may be heated within a range that does not impair the performance, for example, it can be heated to about 40 to 70 ° C. .
- a cleaning method using physical force in combination.
- the removal property of the contamination by the particles adhering to the wiring board 200 is improved, and the cleaning time can be shortened.
- the cleaning method using physical force include scrub cleaning using a cleaning brush and ultrasonic cleaning.
- cleaning with ultrapure water or pure water may be performed before and / or after the cleaning by the cleaning method according to the present embodiment.
- the cleaning method according to the present embodiment when cleaning the wiring board on which the wiring material and the barrier metal material after CMP are coexisted on the surface, corrosion of the wiring material and the barrier metal material is suppressed, and The oxide film and organic residue can be efficiently removed. Further, in the cleaning method according to the present embodiment, as described above, since the cleaning composition that can reduce the corrosion potential difference between copper / cobalt and copper / tantalum nitride is used, copper is used as the wiring material, and cobalt is used as the barrier metal material. In particular, when the wiring substrate coexisting with tantalum nitride is subjected to a cleaning treatment, an excellent effect is exhibited.
- ion-exchanged water and each component shown in Table 1 were placed so that the concentration of the chemical mechanical polishing composition was as shown in Table 1, and stirred for 15 minutes.
- potassium hydroxide and ion-exchanged water are added so that the total amount of all components of the chemical mechanical polishing composition is 100 parts by mass, so that each component has the final concentration and pH shown in Table 1.
- the mixture was filtered through a filter having a pore diameter of 5 ⁇ m to obtain each chemical mechanical polishing composition shown in Table 1.
- the component (A ′) is a component used as a component other than the component (A) described in the claims, instead of the component (A) or in combination with the component (A). is there.
- the film thickness of the cobalt wafer specimen was measured again using a metal film thickness meter “RG-5”, and the difference in film thickness before and after polishing, that is, the film thickness reduced by the chemical mechanical polishing process was calculated.
- the polishing rate was calculated from the reduced film thickness and polishing time.
- the evaluation criteria for the cobalt wafer polishing rate are as follows. The results are also shown in Table 1. A: 100 ⁇ / min or more is judged as a good result. X: Less than 100 kg / min is judged as a bad result.
- the number of defects on the entire surface to be processed was measured for the substrate obtained above using a wafer defect inspection apparatus (KLA 2351, manufactured by KLA Tencor).
- the evaluation criteria are as follows. A: A case where the number of defects on the entire substrate surface (8 inches in diameter) is 250 or less is judged as a good result. X: A case where the number of defects on the entire substrate surface (diameter 8 inches) exceeds 250 is judged as a bad result.
- a measuring device in which an AC tape is controlled by attaching an insulating tape to a 1 ⁇ 1 cm portion of a central portion of a cobalt wafer test piece cut into 1 ⁇ 3 cm and attaching an electrode clip to the exposed area of the upper portion of 1 ⁇ 1 cm. After the immersion for 2.5 minutes, the AC voltage with an amplitude of 5 mV and a frequency of 0.2 MHz-0.05 Hz is reduced from a high frequency. It was applied over the frequency to obtain the real part and imaginary part of the resistance value.
- the semicircular plot obtained by taking the imaginary part on the vertical axis and the real part on the horizontal axis is analyzed by the AC impedance analysis software “ZView” manufactured by Solartron, and the charge transfer resistance ( ⁇ / cm 2 ) is calculated. Calculated.
- the reciprocal of the obtained charge transfer resistance is a value proportional to the corrosion rate of cobalt. If this value is 30,000 or more, it can be judged that the corrosion rate is low.
- Evaluation results Tables 2 and 3 show the compositions and evaluation results of the cleaning compositions.
- the present invention includes substantially the same configuration (for example, a configuration having the same function, method, and result, or a configuration having the same purpose and effect) as the configuration described in the embodiment.
- the invention includes a configuration in which a non-essential part of the configuration described in the embodiment is replaced.
- the present invention includes a configuration that achieves the same effect as the configuration described in the embodiment or a configuration that can achieve the same object.
- the invention includes a configuration in which a known technique is added to the configuration described in the embodiment.
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Abstract
Description
本発明に係る配線基板の化学機械研磨用処理組成物の一態様は、
(A)水溶性アミン、
(B)芳香族炭化水素基を含有する繰り返し単位を有する水溶性重合体、
および水系媒体を含むことを特徴とする。
上記適用例において、
さらに(C)芳香族炭化水素基を有する有機酸を含有することができる。
上記適用例において、
pHが9以上であることができる。
上記適用例において、
前記(A)成分が、アルカノールアミン、ヒドロキシルアミン、モルホリン、モルホリン誘導体、ピペラジン、およびピペラジン誘導体よりなる群から選択される少なくとも1種であることができる。
上記適用例において、
前記(B)成分が、アルキル基置換または非置換のスチレンに由来する構造単位を有する重合体であることができる。
上記適用例において、
前記(C)成分が、フェニルコハク酸、フェニルアラニン、安息香酸、フェニル乳酸、およびナフタレンスルホン酸よりなる群から選択される少なくとも1種であることができる。
上記適用例において、
前記化学機械研磨用処理組成物が、配線基板の被処理面を処理するために用いられ、
前記配線基板は、銅またはタングステンからなる配線材料と、タンタル、チタン、コバルト、ルテニウム、マンガン、およびこれらの化合物よりなる群から選択される少なくとも1種からなるバリアメタル材料と、を被洗浄面に含むことができる。
上記適用例において、
前記被洗浄面は、前記配線材料と前記バリアメタル材料とが接触する部分を含むことができる。
上記適用例において、
前記化学機械研磨用処理組成物が、前記被処理面を洗浄するための洗浄用組成物であることができる。
上記適用例において、
さらに(D)砥粒を含有することができる。
上記適用例において、
前記化学機械研磨用処理組成物が、前記被処理面を研磨するための化学機械研磨用組成物であることができる。
本発明に係る化学機械研磨方法の一態様は、
上記適用例11に記載の化学機械研磨用処理組成物を用いて、前記被処理面を研磨することを特徴とする。
本発明に係る洗浄方法の一態様は、
上記適用例9に記載の化学機械研磨用処理組成物を用いて、前記被処理面を洗浄することを特徴とする。
本発明の一実施形態に係る化学機械研磨用処理組成物は、(A)水溶性アミン(以下「(A)成分」ともいう。)、(B)芳香族炭化水素基を含有する繰り返し単位を有する水溶性重合体(以下「(B)成分」ともいう。)、および水系媒体を含むことを特徴とする。
本実施形態に係る化学機械研磨用処理組成物は、(A)水溶性アミンを含有する。(A)成分は、いわゆるエッチング剤としての機能を有すると発明者は推測する。本実施形態に係る化学機械研磨用処理組成物は、(A)成分を含有することにより、CMPにおける研磨工程、およびCMP終了後における洗浄工程において、配線基板上の金属酸化膜(例えば、CuO、Cu2OおよびCu(OH)2層)や有機残渣(例えばBTA層)をエッチングして除去することができる。
本実施形態に係る化学機械研磨用処理組成物は、(B)芳香族炭化水素基を含有する繰り返し単位を有する水溶性重合体を含有する。(B)成分は、被研磨面の表面に吸着して腐食を低減させる機能を有していると発明者は推測する。そのため、化学機械研磨用処理組成物に(B)成分を添加すると、被処理面の腐食を低減させることができると考えられる。
<分子量測定>
重合体の重量平均分子量(Mw)、数平均分子量(Mn)および分子量分布(Mw/Mn)は、下記条件下で、ゲルパーミエーションクロマトグラフィー法により測定した。
・カラム:東ソー社製カラムの「TSKgel αM」および「TSKgel α2500」を直列に接続。カラムサイズはいずれも7.8×300mm。
・溶媒:0.1Mホウ酸ナトリウム水溶液とアセトニトリルを80対20の割合で混合し、合計100とした水溶液。
・流速:0.8ml/min
・温度:40℃
・検出方法:屈折率法
・標準物質:ポリエチレンオキシド
・GPC装置:東ソー製、装置名「HLC-8020-GPC」
本実施形態に係る化学機械研磨用処理組成物は、(C)芳香族炭化水素基を有する有機酸(以下、「C成分」ともいう。)を含有することができる。(C)成分は、カルボキシ基、スルホ基等の酸性基を1個以上有し、前記酸性基の他に、芳香族炭化水素基を有する化合物である。ただし、重合体は(C)成分には含まないものとする。
本実施形態に係る化学機械研磨用処理組成物を、被処理体を研磨するための化学機械研磨用組成物として用いる場合には、本実施形態に係る化学機械研磨用処理剤は、さらに(D)砥粒を含有することができる。(D)砥粒としては特に限定されないが、具体例としては、シリカ、セリア、アルミナ、ジルコニア、チタニア等の無機粒子が挙げられる。
本実施形態に係る化学機械研磨用処理組成物は、pHが9以上であることが好ましく、10以上14以下であることがより好ましく、10.5以上13.5以下であることがさらに好ましい。pHが9以上である場合には、配線基板表面で上記(B)成分および(C)成分のような保護剤やエッチング剤が機能しやすい状態となるため、良好な被処理面が得られやすくなる。
本実施形態に係る化学機械研磨用処理組成物は、水系媒体を含有する。水系媒体は、水を主成分とした溶媒としての役割を果たすことができるものであれば特に制限されない。このような水系媒体としては、水を用いることがより好ましい。
本実施形態に係る化学機械研磨用処理組成物には、さらにノニオン性界面活性剤を添加してもよい。界面活性剤には、化学機械研磨用処理組成物に適度な粘性を付与する効果がある。化学機械研磨用処理組成物の粘度は、25℃において0.5mPa・s以上2mPa・s以下となるように調製することが好ましい。また、本実施の形態に係る化学機械研磨用処理組成物を洗浄用組成物として用いる場合には、ノニオン性界面活性剤を添加することにより、CMPスラリー中に含まれていたパーティクルや金属不純物を配線基板上から除去する効果が高まり、より良好な被処理面が得られる場合がある。
半導体装置の配線基板では、配線材料とバリアメタル材料とが接触しているため、そこに化学機械研磨用処理組成物が介在すると、電池作用が生じ、各物質固有の電位が卑なる方が選択的に腐食してしまう。しかしながら、本実施形態に係る化学機械研磨用処理組成物を使用した場合には、CMPまたはCMP後の洗浄の際に、(B)成分と(C)成分との相互作用により、配線材料とバリアメタル材料との腐食電位差を小さくすることができるため、ガルバニック腐食を抑制することができると発明者は推測する。
本実施形態に係る化学機械研磨用処理組成物は、化学機械研磨用組成物としてCMPにおいて配線基板を研磨する際に好適に用いることができる。研磨の対象となる配線基板の被研磨面には、銅、コバルトまたはタングステンからなる配線材料と、タンタル、チタン、コバルト、ルテニウム、マンガン、およびこれらの化合物よりなる群から選択される少なくとも1種からなるバリアメタル材料と、を含むことが好ましい。このような配線基板を研磨する場合に、配線材料およびバリアメタル材料の腐食や欠陥の発生を同時に抑制すると共に、研磨速度を低下させることなく、研磨することができる。
本実施形態に係る化学機械研磨用処理組成物の調製方法は、特に制限されないが、例えば(A)成分、(B)成分、必要に応じて(C)成分、(D)成分、ノニオン性界面活性剤を、水系媒体に添加して撹拌・混合することにより各成分を水系媒体に溶解させ、次にpH調整剤を添加して所定のpHに調整する方法が挙げられる。pH調整剤以外の各成分の混合順序や混合方法については特に制限されない。
本実施形態に係る化学機械研磨または洗浄方法は、上述の化学機械研磨用処理組成物を用いて化学機械研磨または洗浄する工程を含むことを特徴とする。本実施形態に係る化学機械研磨または洗浄方法は特に限定されないが、一具体例について、図面を用いながら以下詳細に説明する。
本実施形態に係る化学機械研磨または洗浄方法を実施する配線基板は、凹部が形成された絶縁膜と、前記凹部内の底面ないし側面を覆うようにして形成されたバリアメタル膜と、前記バリアメタル膜を覆うようにして前記凹部に埋め込まれ、配線となる金属酸化膜と、を備える。この配線基板において、バリアメタル膜の材料が、タンタル、チタン、コバルト、ルテニウム、マンガン、およびこれらの化合物よりなる群から選択される少なくとも1種を含むものであり、凹部に埋め込まれ金属酸化膜が、銅またはタングステンを含む。この配線基板は、次に説明するように、被処理体を、化学機械研磨用組成物を用いた化学機械研磨することで得られる。
図1は、化学機械研磨に用いられる被処理体を模式的に示した断面図である。まず、図1に示す被処理体100の製造方法について説明する。
本実施形態において、化学機械研磨は、被研磨体を研磨パッドに圧着し、研磨パッド上に化学機械研磨用組成物を供給しながら被研磨体と研磨パッドとを相互に摺動させて、被研磨体を化学的かつ機械的に研磨する技術である。
・定盤回転数;好ましくは30~120rpm、より好ましくは40~100rpm
・ヘッド回転数;好ましくは30~120rpm、より好ましくは40~100rpm
・定盤回転数/ヘッド回転数比;好ましくは0.5~2、より好ましくは0.7~1.5
・研磨圧力;好ましくは60~200gf/cm2、より好ましくは100~150gf/cm2
・化学機械研磨用処理組成物供給速度;好ましくは50~400mL/分、より好ましくは100~300mL/分
次いで、図3に示す配線基板200の表面(被洗浄面200a)を上述の洗浄用組成物を用いて洗浄する。図3に示すように、被洗浄面200aは、配線材料である金属酸化膜16とバリアメタル材料によって形成されたバリアメタル膜14とが接触する部分も含む。
以下、本発明を実施例により説明するが、本発明はこれらの実施例により何ら限定されるものではない。なお、本実施例における「部」および「%」は、特に断らない限り質量基準である。
3.1.1.化学機械研磨用組成物の調製
ポリエチレン製容器に、イオン交換水と、表1に示す各成分を化学機械研磨用組成物としての濃度が表1になるように入れ、15分間撹拌した。この混合物に、水酸化カリウムとイオン交換水を、化学機械研磨用組成物の全構成成分の合計量が100質量部となるように加えて各成分が表1に示す最終濃度、pHとなるように調整した後、孔径5μmのフィルターで濾過して、表1に示す各化学機械研磨用組成物を得た。なお、表1において、(A’)成分とは、請求の範囲に記載の(A)成分以外の成分として、(A)成分の代わりに、もしくは(A)成分と併用して用いた成分である。(B’)成分についても同様である。
3.1.2.1.研磨速度の評価
コバルトウエハ試験片をNPS株式会社製、金属膜厚計「RG-5」を用いて予め膜厚を測定し、研磨装置としてラップマスターSFT社製、型式「LM-15C」、研磨パッドとしてロデール・ニッタ株式会社製、「IC1000/K-Groove」を用い、定盤回転数90rpm、ヘッド回転数90rpm、ヘッド押し付け圧3psi、化学機械研磨用組成物供給速度100mL/分の研磨条件で1分間化学機械研磨処理(CMP)した。研磨処理後に再び金属膜厚計「RG-5」を用いてコバルトウエハ試験片の膜厚を測定し、研磨前後の膜厚の差、すなわち化学機械研磨処理により減少した膜厚を算出した。減少した膜厚および研磨時間から研磨速度を算出した。コバルトウエハ研磨速度の評価基準は下記の通りである。その結果を表1に併せて示す。
○:100Å/min以上を良好な結果と判断する。
×:100Å/min未満を悪い結果と判断する。
シリコン基板上にコバルト膜を厚さ2000Å積層させた8インチウエハを、化学機械研磨装置「EPO112」(株式会社荏原製作所製)を用いて、下記の条件で化学機械研磨を実施した。
・化学機械研磨用組成物種:表1に示した化学機械研磨用組成物
・研磨パッド:ロデール・ニッタ(株)製、「IC1000/SUBA400」
・定盤回転数:70rpm
・ヘッド回転数:70rpm
・ヘッド荷重:250g/cm2
・化学機械研磨用組成物供給速度:200mL/分
・研磨時間:60秒
<ブラシスクラブ洗浄>
・洗浄剤:和光純薬工業(株)製、「CLEAN-100」
・上部ブラシ回転数:100rpm
・下部ブラシ回転数:100rpm
・基板回転数:100rpm
・洗浄剤供給量:300mL/分
・洗浄時間:30秒
○:基板表面(直径8インチ)全体における欠陥数が250個以下である場合を良好な結果であると判断する。
×:基板表面(直径8インチ)全体における欠陥数が250個を超える場合を悪い結果であると判断する。
上記3.1.2.2.で得られた基板表面を光学顕微鏡で観察し、基板表面のdot数を計測することにより腐食の評価を行った。評価基準は下記の通りである。その結果を表1に併せて示す。
○:基板表面(直径8インチ)全体におけるdot数が20個以下である場合を良好な結果であると判断する。
×:基板表面(直径8インチ)全体におけるdot数が20個を超える場合を悪い結果であると判断する。
化学機械研磨用組成物の組成、および評価結果を下表1に示す。
・スチレン-マレイン酸共重合体(第一工業製薬社製、商品名DKSディスコートN-10、Mw=3200)
・スチレン-マレイン酸ハーフエステル共重合体(第一工業製薬社製、商品名DKSディスコートN-14,Mw=3600)
・ナフタレンスルホン酸ホルマリン縮合物(第一工業製薬社製、商品名ラベリンFD-40、Mw=2700)
・ポリアクリル酸(東亜合成社製、商品名ジュリマーAC-10H、Mw=700,000)
3.2.1.洗浄用組成物の調製
ポリエチレン製容器に、イオン交換水と、表2または表3に示す水酸化カリウム以外の各成分を洗浄用組成物としての濃度が表2または表3になるように入れ、15分間撹拌した。この混合物に、水酸化カリウムとイオン交換水を全構成成分の合計量が100質量部となるように加えて表2または表3に示すpHとなるように調整した。その後、孔径5μmのフィルターで濾過して、表2または表3に示す各洗浄用組成物を得た。pHは、株式会社堀場製作所製のpHメーター「F52」を用いて測定した。なお、表2、3において、(B’)成分とは、請求の範囲に記載の(B)成分以外の成分として、(B)成分の代わりに、もしくは(B)成分と併用して用いた成分である。
3.2.2.1.化学機械研磨
シリコン基板上にコバルト膜を厚さ2000Å積層させた8インチウエハを、化学機械研磨装置「EPO112」(株式会社荏原製作所製)を用いて、下記の条件で化学機械研磨を実施した。
・化学機械研磨用組成物種:JSR(株)製、「CMS7501/CMS7552」
・研磨パッド:ロデール・ニッタ(株)製、「IC1000/SUBA400」
・定盤回転数:70rpm
・ヘッド回転数:70rpm
・ヘッド荷重:50g/cm2
・化学機械研磨用組成物供給速度:200mL/分
・研磨時間:60秒
上記化学機械研磨に続いて、研磨後の基板表面を、下記の条件で定盤上洗浄し、さらにブラシスクラブ洗浄した。
<定盤上洗浄>
・洗浄剤:上記で調製した洗浄用組成物
・ヘッド回転数:70rpm
・ヘッド荷重:100g/cm2
・定盤回転数:70rpm
・洗浄用組成物供給速度:300mL/分
・洗浄時間:30秒
<ブラシスクラブ洗浄>
・洗浄剤:上記で調製した洗浄用組成物
・上部ブラシ回転数:100rpm
・下部ブラシ回転数:100rpm
・基板回転数:100rpm
・洗浄用組成物供給量:300mL/分
・洗浄時間:30秒
3.2.3.1.欠陥評価
上記3.2.2.2.で得られた洗浄後の基板表面をウエハ欠陥検査装置(ケーエルエー・テンコール社製、KLA2351)を用いて、被研磨面全面の欠陥数を計測した。評価基準は下記の通りである。その結果を表2または表3に併せて示す。
○:基板表面(直径8インチ)全体における欠陥数が250個以下である場合に良好な結果と判断する。
×:基板表面(直径8インチ)全体における欠陥数が250個を超える場合を悪い結果と判断する。
上記3.2.2.2.で得られた洗浄後の基板表面を光学顕微鏡で観察し、基板表面のdot数を計測観察することにより腐食の評価を行った。評価基準は下記の通りである。その結果を表2または表3に併せて示す。
○:基板表面(直径8インチ)全体におけるdot数が20個以下である場合に良好な結果と判断する。
×:基板表面(直径8インチ)全体におけるdot数が20個を超える場合を悪い結果と判断する。
測定装置として、ポテンショ/ガルバノスタット(ソーラトロン社製、SI 1287)に周波数応答アナライザ(ソーラトロン社製、1252A型FRA)を接続して用い、一端を水溶液に浸漬したコバルトウエハ試験片に振幅5mV、周波数0.2MHz-0.05Hzの交流電圧を高周波から低周波にかけて印加し、抵抗値を得た。より詳細には、1×3cmにカットしたコバルトウエハ試験片中央部1×1cmの部位に絶縁テープを貼り、その上部1×1cmの露出領域に電極クリップを取り付けて交流電圧が制御された測定装置に接続し、下部1×1cmの露出領域を得られた洗浄用組成物に浸漬し、浸漬2.5分経過した後に、振幅5mV、周波数0.2MHz-0.05Hzの交流電圧を高周波から低周波にかけて印加し、抵抗値の実部と虚部の値を得た。縦軸に虚部、横軸に実部を取ることにより得られた半円状のプロットを、ソーラトロン社製の交流インピーダンス解析ソフト「ZView」により解析し、電荷移動抵抗(Ω/cm2)を算出した。なお、得られた電荷移動抵抗の逆数は、コバルトの腐食速度に比例する値である。この値が30,000以上であれば、腐食速度が低いと判断できる。
表2および表3に、洗浄用組成物の組成および評価結果を示す。
・スチレン-マレイン酸共重合体(第一工業製薬社製、商品名DKSディスコートN-10、Mw=3200)
・ナフタレンスルホン酸ホルマリン縮合物(第一工業製薬社製、商品名ラベリンFD-40、Mw=2700)
・ポリアクリル酸(東亜合成社製、商品名ジュリマーAC-10H、Mw=700,000)
Claims (13)
- (A)水溶性アミン、
(B)芳香族炭化水素基を含有する繰り返し単位を有する水溶性重合体、
および水系媒体を含む、化学機械研磨用処理組成物。 - さらに(C)芳香族炭化水素基を有する有機酸を含有する、請求項1に記載の化学機械研磨用処理組成物。
- pHが9以上である、請求項1または請求項2に記載の化学機械研磨用処理組成物。
- 前記(A)成分が、アルカノールアミン、ヒドロキシルアミン、モルホリン、モルホリン誘導体、ピペラジン、およびピペラジン誘導体よりなる群から選択される少なくとも1種のアミノ酸である、請求項1ないし請求項3のいずれか一項に記載の化学機械研磨用処理組成物。
- 前記(B)成分が、アルキル基置換または非置換のスチレンに由来する構造単位を有する重合体である、請求項1ないし請求項4のいずれか一項に記載の化学機械研磨用処理組成物。
- 前記(C)成分が、フェニルコハク酸、フェニルアラニン、安息香酸、フェニル乳酸およびナフタレンスルホン酸よりなる群から選択される少なくとも1種である、請求項2ないし請求項5のいずれか一項に記載の化学機械研磨用処理組成物。
- 前記化学機械研磨用処理組成物が、配線基板の被処理面を処理するために用いられ、
前記配線基板は、銅またはタングステンからなる配線材料と、タンタル、チタン、コバルト、ルテニウム、マンガン、およびこれらの化合物よりなる群から選択される少なくとも1種からなるバリアメタル材料と、を前記被処理面に含む、請求項1ないし請求項6のいずれか一項に記載の化学機械研磨用処理組成物。 - 前記被処理面は、前記配線材料と前記バリアメタル材料とが接触する部分を含む、請求項7に記載の化学機械研磨用処理組成物。
- 前記化学機械研磨用処理組成物が、前記被処理面を洗浄するための洗浄用組成物である、請求項7または請求項8に記載の化学機械研磨用処理組成物。
- さらに(D)砥粒を含有する、請求項1ないし請求項8のいずれか一項に記載の化学機械研磨用組成物。
- 前記化学機械研磨用処理組成物が、前記被処理面を研磨するための化学機械研磨用組成物である、請求項10に記載の化学機械研磨用処理組成物。
- 請求項11に記載の化学機械研磨用処理組成物を用いて、前記被処理面を研磨する、化学機械研磨方法。
- 請求項9に記載の化学機械研磨用処理組成物を用いて、前記被処理面を洗浄する、洗浄方法。
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JP2019108462A (ja) * | 2017-12-18 | 2019-07-04 | 花王株式会社 | ハードディスク用基板用の洗浄剤組成物 |
Also Published As
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KR20170134963A (ko) | 2017-12-07 |
CN107210214A (zh) | 2017-09-26 |
TW201700662A (zh) | 2017-01-01 |
US20180086943A1 (en) | 2018-03-29 |
TWI751969B (zh) | 2022-01-11 |
JPWO2016158648A1 (ja) | 2018-03-01 |
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