WO2007077886A1 - 金属用研磨液及び被研磨膜の研磨方法 - Google Patents
金属用研磨液及び被研磨膜の研磨方法 Download PDFInfo
- Publication number
- WO2007077886A1 WO2007077886A1 PCT/JP2006/326106 JP2006326106W WO2007077886A1 WO 2007077886 A1 WO2007077886 A1 WO 2007077886A1 JP 2006326106 W JP2006326106 W JP 2006326106W WO 2007077886 A1 WO2007077886 A1 WO 2007077886A1
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- Prior art keywords
- polishing
- metal
- acid
- polished
- polishing liquid
- Prior art date
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- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229960002510 mandelic acid Drugs 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- IYRGXJIJGHOCFS-UHFFFAOYSA-N neocuproine Chemical compound C1=C(C)N=C2C3=NC(C)=CC=C3C=CC2=C1 IYRGXJIJGHOCFS-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 229940116315 oxalic acid Drugs 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000008363 phosphate buffer Substances 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920002800 poly crotonic acid Polymers 0.000 description 1
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 1
- 229920001798 poly[2-(acrylamido)-2-methyl-1-propanesulfonic acid] polymer Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 108010064470 polyaspartate Proteins 0.000 description 1
- 229920002643 polyglutamic acid Polymers 0.000 description 1
- 229920000656 polylysine Polymers 0.000 description 1
- 229920001444 polymaleic acid Polymers 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229940005642 polystyrene sulfonic acid Drugs 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 description 1
- ROSDSFDQCJNGOL-UHFFFAOYSA-N protonated dimethyl amine Natural products CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 125000005372 silanol group Chemical group 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229940032330 sulfuric acid Drugs 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229960001367 tartaric acid Drugs 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910021654 trace metal Inorganic materials 0.000 description 1
- VZZUPGZLDMTMFL-UHFFFAOYSA-N triazine;trithiole Chemical compound S1SC=CS1.C1=CN=NN=C1 VZZUPGZLDMTMFL-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—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]
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
Definitions
- the present invention relates to a metal polishing liquid and a polishing method for a film to be polished.
- CMP chemical mechanical polishing
- a general method of CMP of metal is to apply a polishing pad on a circular polishing platen (platen), immerse the polishing pad surface with a metal polishing liquid, and press the surface on which the metal film of the substrate is formed.
- the polishing platen is turned with a predetermined pressure (hereinafter referred to as polishing pressure) applied from the back surface, and the metal film on the convex portion is formed by mechanical friction between the polishing liquid and the convex portion of the metal film. It will be removed.
- Metal polishing liquids used in CMP generally have an oxidizing agent and abrasive particle force, and a metal oxide solubilizer, a metal anticorrosive, and the like are further added as necessary.
- the basic mechanism is to oxidize the surface of the metal film by oxidation and scrape the oxide layer with abrasive particles. Since the oxide layer on the metal surface of the recess does not touch the polishing pad so much and the effect of polishing off by the abrasive particles is not exerted, the metal layer of the projection is removed with the progress of CMP, and the substrate surface is flattened.
- Journal 'Ob' Elect Mouth Chemical See Society 138-11 (published in 1991), pages 3460-3464).
- a metal oxide solubilizer made of aminoacetic acid or amide sulfate such as glycine is used to suppress the occurrence of dishing, erosion and polishing flaws and to form LSI wiring with high reliability.
- a method of using a metal polishing liquid containing a protective film forming agent such as BTA (benzotriazole) has been proposed (see, for example, JP-A-8-83780).
- BTA benzotriazole
- a method for solving the poor flatness due to the effect of forming a protective film such as BTA may be unfavorable because the force polishing rate that can suppress the occurrence of dating and erosion is significantly reduced.
- removal of abrasive particles adhering to the substrate by CMP treatment is mainly performed by physical cleaning with a polyvinyl alcohol brush or ultrasonic waves.
- abrasive particles adhering to the substrate become finer, it becomes difficult to effectively apply physical force to the abrasive particles.
- a polishing liquid for metal films particularly copper or a metal mainly composed of copper
- a polishing liquid substantially free of abrasive particles is disclosed in, for example, Japanese Patent No. 3371775.
- a buried metal wiring can be formed by applying mechanical friction to the metal surface using a polishing liquid containing a film forming agent.
- a method of forming a copper wiring with a polishing solution containing substantially no abrasive particles containing hydrogen peroxide, citrate, and benzotriazole is described as an example, and the above-mentioned (a) to (d) The problem has been solved.
- the polishing rate under normal polishing conditions is 80 to 150 nmZ and 300 gZcm 2 or more. There is a problem that the polishing rate is saturated and does not exceed 200 nmZ even when a polishing load is applied.
- polishing flaws, erosion, and the need for removal of polishing barrels after polishing with a metal-polishing liquid that does not contain polishing barrels or that contains a very small amount of polishing barrels problems such as the cost of the grains themselves and cost increase due to waste liquid treatment, and the problem of polishing speed for the purpose of improving throughput can be solved, but it is difficult to reduce dating that greatly contributes to wiring reliability and performance Met.
- the present invention removes abrasive particles remaining on the substrate surface after polishing, (a) generation of polishing flaws derived from solid particles, (b) generation of flatness such as dating and erosion, etc. (D) Metal polishing liquid that can be CMPed at a high Cu polishing rate, and solves problems such as the complexity of the cleaning process, (d) the cost of solid abrasive grains itself and the cost increase caused by waste liquid treatment.
- the present invention provides a metal polishing liquid capable of forming a buried Cu wiring at a level of 130 nm or more at a technology node and a polishing method for a film to be polished using the same.
- the present invention comprises (1) a metal oxidant, a metal oxide solubilizer, a metal anticorrosive, and a water-soluble polymer having a ionic functional group having a weight average molecular weight of 8,000 or more, and a pH
- the present invention relates to a metal-polishing liquid characterized in that is 1 or more and 3 or less.
- the present invention provides (2) one or more kinds wherein the metal oxidizing agent is selected from hydrogen peroxide, ammonium persulfate, nitric acid, potassium periodate, hypochlorous acid, and ozone hydraulic power.
- the metal oxidizing agent is selected from hydrogen peroxide, ammonium persulfate, nitric acid, potassium periodate, hypochlorous acid, and ozone hydraulic power.
- the present invention provides (3) an inorganic acid, an organic acid, or a salt thereof, wherein the metal oxide solubilizer has a first-stage acid dissociation constant of less than 3.7 at 25 ° C.
- the present invention also provides: (4) the metal oxide solubilizer is malonic acid, citrate, malic acid, glycolic acid, glutamic acid, glyconic acid, oxalic acid, tartaric acid, picolinic acid, nicotinic acid, mande It is one or more metal oxide solubilizers selected from phosphoric acid, acetic acid, sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, formic acid, lactic acid, phthalic acid, fumaric acid, maleic acid, aminoacetic acid, amidosulfuric acid and salts thereof
- the present invention relates to the metal polishing slurry according to any one of (1) to (3).
- the present invention provides (5) wherein the metal anticorrosive is at least one metal anticorrosive selected from nitrogen-containing cyclic compounds and ionic surfactants.
- the metal polishing slurry according to any one of the above.
- the present invention provides: (6) the water-soluble polymer having a terionic functional group is at least one anionic functional group of a sulfonic acid group, a carboxylic acid group, a phosphoric acid group, or a salt thereof.
- the metal-polishing liquid according to any one of (1) to (5), wherein the metal-polishing liquid is a water-soluble polymer.
- the present invention is as described in any one of (1) to (6) above, wherein (7) less than 1% by weight of abrasive particles is added to the weight of the metal polishing slurry.
- This relates to a metal polishing slurry.
- the present invention is also characterized in that (8) the abrasive particles are one or more types of abrasive particles selected from silica, alumina, ceria, titer, zirconium, germania force. 1 ) To (7).
- the present invention relates to the metal polishing slurry according to one item.
- the present invention is also characterized in that (9) the metal to be polished which is an object to be polished by the metal polishing liquid is at least one metal selected from copper, a copper alloy and a copper compound.
- Any one of (1) to (8) is related to the metal polishing liquid according to one item.
- the present invention provides (10) a film to be polished while supplying the metal polishing liquid according to any one of (1) to (9) above on a polishing cloth of a polishing surface plate.
- a polishing method for a film to be polished is characterized in that polishing is performed by relatively driving the polishing platen and the substrate while the substrate is pressed against the polishing cloth.
- the above problems (a) to (d) can be solved, and low dishing, that is, technology one at a high polishing rate. It is possible to form embedded Cu wiring at the level required after node 130nm.
- Figure 1 shows the relationship between pH and polymer diameter of an aqueous solution in which the water-soluble polymer having an anionic functional group is polycarboxylic acid and the metal oxide solubilizer is sulfuric acid, and the metal oxidizer is peroxidized. This is a graph plotting the relationship between ⁇ and dating of a metal polishing slurry in which hydrogen, a metal oxide solubilizer is sulfuric acid, a metal anticorrosive is benzotriazole, and a water-soluble polymer having an ionic functional group is a polycarboxylic acid. is there.
- the present inventors in a sufficiently low pH range, have a metal anticorrosive and a weight average.
- a water-soluble polymer having an ionic functional group with an average molecular weight of 8,000 or more By using a water-soluble polymer having an ionic functional group with an average molecular weight of 8,000 or more, a sufficiently high polishing rate applicable to CMP can be achieved, and the level required after Technology Node 130 ⁇ m We found that it was possible to form embedded Cu wiring with the amount of dicing.
- the metal polishing slurry of the present invention contains a metal oxidizer, a metal oxide solubilizer, a metal anticorrosive, and a water-soluble polymer having an anionic functional group having a weight average molecular weight of 8,000 or more, p H is 1 or more and 3 or less.
- the pH of the metal polishing slurry of the present invention is 1 or more and 3 or less, preferably 1.5 or more and 2. 8 or less, and more preferably 1.8 or more and 2.5 or less.
- the pH can be adjusted by, for example, the amount of metal oxide solubilizer added to the metal polishing slurry. It is also possible to adjust by using a base such as ammonia or potassium hydroxide in combination with a metal oxide solubilizer.
- the pH in the present invention can be measured with a pH meter (for example, Model pH81, manufactured by Yokogawa Electric Corporation).
- the measurement method consists of two points using a standard buffer (phthalate pH buffer pH: 4.21 (25 ° C), neutral phosphate pH buffer pH 6.86 (25 ° C). The value after the electrode was put in the polishing liquid and stabilized after 2 minutes or more was defined as the pH of the polishing liquid.
- Examples thereof include ammonium, ammonium persulfate, hypochlorous acid, and ozone water.
- hydrogen peroxide is preferred.
- These oxidizing agents can be used alone or in combination of two or more. If the substrate is a silicon substrate containing integrated circuit elements, contamination by alkali metals, alkaline earth metals, halides, etc. is not desirable. Therefore, an oxidant that does not contain non-volatile components is the most desirable aspect of stability. Preference is given to hydrogen peroxide and hydrogen peroxide.
- the blending amount of the oxidizing agent in the present invention is appropriately selected, but it is preferably 3 to 20% by weight and more preferably 5 to 15% by weight with respect to the total weight of the polishing liquid. When the blending amount of the oxidizing agent is less than 3% by weight, a sufficient polishing rate tends not to be obtained, and when it exceeds 20% by weight, a sufficient polishing rate tends not to be obtained.
- the metal oxide solubilizer in the present invention has an inorganic acid or organic acid whose first-stage acid dissociation index (pKl) at 25 ° C is preferably less than 3.7, more preferably 2.0 to 3.7. One or more water-soluble acid / metal solubilizers selected from acids or their salts.
- malic acid, citrate, malic acid, glycolic acid, glutamic acid, daliconic acid, oxalic acid, tartaric acid, picolinic acid, nicotinic acid, mandelic acid, acetic acid, sulfuric acid examples thereof include nitric acid, phosphoric acid, hydrochloric acid, formic acid, lactic acid, phthalic acid, fumaric acid, maleic acid, aminoacetic acid, amidosulfuric acid, and its ammonium salt and potassium salt.
- metal oxide solubilizers are preferable in that a balance with the protective curtain forming agent is easily obtained.
- malic acid, tartaric acid, citrate, phosphoric acid, and sulfuric acid are preferred because malic acid, tartaric acid, citrate, phosphoric acid, and sulfuric acid are preferred because the etching rate can be effectively suppressed while maintaining a practical CMP rate. Is more preferable.
- These metal oxide solubilizers can be used alone or in combination of two or more.
- the present invention it is necessary to suppress dissociation of the ionic functional group of the water-soluble polymer in order to achieve high polishing rate and low dicing. It is effective to add an acid having a low acid dissociation index in the first stage in order to suppress the dissociation of the char-on functional group. Specifically, the acid dissociation index in the first stage is less than 3.7. It has been found that a certain water-soluble metal oxide solubilizer is useful for suppressing the dissociation of the water-soluble polymer's ionic functional group.
- the acid dissociation index in the present invention is a logarithmic value of the reciprocal of the acid dissociation constant. For example, the 4th edition of “Basic Study Guide for Basic Studies” (issued on September 30, 1993), Maruzen Co., Ltd. — Detailed description on pages 317-321
- the compounding amount of the metal oxide solubilizer in the present invention is appropriately selected, but is preferably 0.05 to 3.0% by weight with respect to the total weight of the polishing liquid. More preferably, it is 0% by weight.
- the blending amount of the metal oxide solubilizer is less than 0.05% by weight, a sufficient polishing speed tends to be not obtained, and when it exceeds 3.0% by weight, practical flatness is obtained. There is no tendency.
- the metal anticorrosive in the present invention is considered to form a protective film on the oxide layer on the surface of the metal film and prevent dissolution of the acid layer in the polishing liquid.
- ammonia dimethylamine Alkylamines such as trimethylamine, triethylamine and propylenediamine, Amines such as range amine tetraacetic acid (EDTA), sodium jetyldithiocarbamate, chitosan, etc .
- dithizone cuproin (2,2'-biquinoline), neocuproine (2,9 dimethyl-1,10 phenanthorin) 2, 9 Dimethinore 4, 7 Diphenol 1, 10-phenantorin), cuperazone (biscyclohexanone oxalylhydrazone), etc .
- benzimidazole 2-thiol triazine dithiol, triazine trithiol, 2- [2- (Benzothiazolyl)] thiopropionic acid, 2- [
- nitrogen-containing cyclic compounds and ionic surfactants are suitable for reducing the etching rate and achieving high polishing rate, and nitrogen-containing cyclic compounds are more preferred.
- an ionic surfactant an ion whose ionic group has one or more of sulfonic acid group, carboxylic acid group, phosphoric acid group, and phenolic hydroxyl group, and whose hydrophobic group has 6 or more carbon atoms.
- a surfactant is preferred.
- the compounding amount of the metal anticorrosive in the present invention is appropriately selected, but it is preferably 0.05 to 3.0% by weight with respect to the total weight of the polishing liquid. It is better to have it.
- the amount of the metal anticorrosive is less than 0.05% by weight, sufficient anticorrosive effect cannot be obtained, and etching tends to increase and the flatness tends to deteriorate. In this case, there is a tendency that a practical polishing rate cannot be obtained.
- the weight average molecular weight of the water-soluble polymer having an anionic functional group in the present invention is 8,000 or more, preferably ⁇ is 8,000 or more and 200,000 or less, and more preferably ⁇ is 20,000 or more and 100. , 000 or less, particularly preferably 40,000 or more and 80,000 or less.
- the upper limit of the weight average molecular weight is not particularly limited. For example, if it exceeds 200,000, no significant decrease in the polishing rate is observed, but there is a large variation in the polishing rate distribution within the polished wafer surface. As a result, dating tends to increase.
- the weight average molecular weight of the water-soluble polymer having an anionic functional group in the present invention was measured by gel permeation chromatography. The measurement conditions are as shown below.
- the water-soluble polymer having a ergonal functional group is a water-soluble polymer having at least one of a sulfonic acid group, a carboxylic acid group, a phosphoric acid group, or a salt thereof.
- a sulfonic acid group, a carboxylic acid group, and a phosphoric acid group are preferable, and a sulfonic acid group and a carboxylic acid group are more preferable.
- the salt include an alkali metal salt, an alkaline earth metal salt, a halide, and an ammonium salt.
- the substrate to which the polishing liquid is applied is a silicon substrate for a semiconductor integrated circuit, etc.
- Water-soluble polymers having a strong ionic group include polystyrene sulfonic acid, polyacrylamidomethylpropane sulfonic acid, polymalic acid, polyacrylic acid, polymethacrylic acid, polycrotonic acid, polyitaconic acid, polymaleic acid, polyfumaric acid.
- polycarboxylic acids examples thereof include acids, polyvinyl sulfonic acid, polyaspartic acid, polyglutamic acid, polyphosphoric acid, polymetaphosphoric acid, or ammonium salts, alkali metal salts, alkaline earth metal salts thereof, and the like.
- polycarboxylic acids are used for prizes.
- the polycarboxylic acid refers to a water-soluble polymer having a powerful oxyl group as a functional group.
- a high polishing rate and good dating can be obtained by adding a water-soluble polymer having a ergonal functional group.
- the amount of the water-soluble polymer to be used is suitably selected. It is preferably 0.05 to 2.0% by weight, based on the total weight of the polishing liquid, and 0.1 to 0.8% by weight. It is more preferable.
- the blending amount of the water-soluble polymer having a ergonal functional group is less than 0.05% by weight, it is in the “tilt port where a practical polishing rate cannot be obtained”.
- Fig. 1 shows the relationship between pH and the particle size and dishing of water-soluble polymers with key functional groups.
- the particle size of the water-soluble polymer having an anionic functional group was measured by adjusting the pH of the water-soluble polymer having an anionic functional group with the addition amount of an acid metal dissolving agent.
- the water-soluble polymer having a eron functional group was a polycarboxylic acid, and sulfuric acid was used as the metal oxide solubilizer.
- Dating is also a water-soluble polymer having a metal oxidizer, metal oxide solubilizer, metal anticorrosive, and char-on functional group, and its pH is adjusted by the amount of acid metal solubilizer added.
- the metal oxidant is hydrogen peroxide
- the metal oxide solubilizer is sulfuric acid
- the metal anticorrosive is benzotriazole
- the water-soluble polymer having a ionic functional group is polycarboxylic acid.
- the particle size of the water-soluble polymer having a ergonal functional group is a value obtained by a laser diffraction particle size distribution meter, and is taken as a guideline indicating the spread of the polymer chain in an aqueous solution.
- the particle size shown is the median diameter. The lower the pH, the smaller the polymer diameter. I understand.
- the protective film formed on the metal to be polished is a metal anticorrosive or polymer adsorbing layer in the metal polishing liquid, or a metal anticorrosive or polymer and the metal to be polished or its ions are coordinated or ion-bonded. It is considered a layer of reactants bound by covalent bonds or the like.
- the metal anticorrosive is very effective in suppressing dishing because it forms a dense and strong protective film, but the polishing rate is lowered by increasing the amount of addition.
- the metal polishing liquid to which a water-soluble polymer is added reduces the effect of suppressing the increase in force dating that can avoid a decrease in the polishing rate. This exists in a state where the water-soluble polymer chain is extended in the metal polishing liquid, and the protective film formed by this polymer chain becomes a rough protective film, which reduces the effect of suppressing the increase in dating. it is conceivable that.
- the metal-polishing liquid of the present invention has a dense water-soluble polymer in which polymer chains are shrunk by using a low pH region, that is, a dense water-soluble polymer efficiently coats the metal to be polished. It is believed that a protective film is formed to suppress the increase in dateing.
- the polishing speed is increased, but it becomes difficult to obtain flatness of the surface to be polished.
- the polymer molecular weight is small, flatness of the surface to be polished is obtained, but polishing is difficult. It tends to be slow.
- polishing speed and flatness of the surface to be polished can be achieved.
- a high polishing rate has been achieved by forming a soft protective film that is denser than a strong protective film such as a metal anticorrosive.
- a metal anticorrosive and a water-soluble polymer together, a soft protective film is formed compared to using the metal anticorrosive alone; W polishing speed is improved, but flatness of the polished surface is not obtained .
- a specific pH region using a metal anticorrosive and a water-soluble polymer having a weight average molecular weight of 8000 or more a high polishing rate and flatness of the surface to be polished can be achieved.
- the water-soluble polymer in an aqueous solution adjusted in pH with an acid-metal solubilizer used in the present invention was measured with a laser diffraction particle size distribution meter.
- Measuring device ZETASIZER3000HS manufactured by MALVERN
- the polishing rate can be further improved by adding abrasive particles which may be added to the metal polishing slurry.
- the amount of abrasive particles added is appropriately selected within a range that does not affect the effects of the present invention.
- the amount of abrasive particles added is preferably less than 1% by weight, more preferably 0.001 to 1% by weight, and particularly preferably 0.03 to 1% by weight, based on the weight of the polishing liquid.
- the lower limit of the addition amount of the abrasive particles is not particularly limited. For example, if it is less than 0.001% by weight, the addition effect tends not to be expected without contributing to the improvement of the polishing rate.
- abrasive particles for example, inorganic abrasive grains such as silica, alumina, titer, ceria, zircoure, germania, etc., organic abrasive grains such as polystyrene, polyacryl, polyvinyl chloride vinyl and the like can be mentioned.
- organic abrasive grains such as polystyrene, polyacryl, polyvinyl chloride vinyl and the like
- colloidal silica and Z or colloidal silica which are preferred to silica, alumina and ceria, are more preferred.
- colloidal silica refers to those based on colloidal silica, with a small amount of metal species added during the sol-gel reaction, and those with surface silanol groups chemically modified, etc. There is no. These abrasive particles can be used alone or in combination of two or more.
- the primary particle size of the abrasive particles is a force that is appropriately adjusted according to the type of metal to be polished, the type of abrasive particles, etc., preferably 200 nm or less, more preferably 5 to 200 nm, particularly preferably 5 to 150 nm, and most preferably Is 5 to 100 nm.
- the primary particle size exceeds 200 nm, the flatness of the polished surface tends to deteriorate. Care should be taken when selecting a primary particle size of less than 5 nm as the CMP rate may be reduced.
- the secondary particle diameter is preferably 200 nm or less, more Preferably it is 10-200 nm, Especially preferably, it is 10-150 nm, Most preferably, 10-: LOOnm.
- the secondary particle diameter exceeds 200 nm, the flatness of the polished surface tends to deteriorate.
- care must be taken because the mechanical reaction layer removal capability of abrasive particles is insufficient and the CMP rate may be reduced.
- the primary particle diameter of the abrasive particles in the present invention can be measured using a transmission electron microscope (for example, S4700 manufactured by Hitachi, Ltd.).
- the secondary particle diameter can be measured using a light diffraction / scattering particle size distribution analyzer (for example, COULTER N4SD manufactured by COULTER Electronics).
- the metal polishing liquid of the present invention contains additives generally added to the polishing liquid, such as colorants such as dyes and pigments, pH adjusters, and solvents other than water. It may be added in a range without impairing the action and effect of the polishing liquid.
- the method for polishing a film to be polished according to the present invention comprises a substrate having a metal film to be polished pressed against the polishing cloth while supplying the metal polishing liquid of the present invention onto the polishing cloth of a polishing surface plate. It is characterized in that the metal film to be polished is polished by relatively driving the polishing surface plate and the substrate.
- the metal film to be polished which is an object to be polished, may be a single layer or a multilayer.
- the metal film include one or more of metals such as copper, aluminum, tungsten, tantalum, and titanium, alloys of these metals, and oxides and nitrides of these metals or metal alloys. Among these, copper, a copper alloy, and a copper compound are preferable.
- the metal film is formed by a known method such as a sputtering method or a plating method.
- an insulating layer is formed on a semiconductor substrate such as a substrate for manufacturing a semiconductor device, for example, a semiconductor substrate at a stage where a circuit element and a wiring pattern are formed, or a semiconductor substrate at a stage where a circuit element is formed.
- a semiconductor substrate such as a substrate for manufacturing a semiconductor device, for example, a semiconductor substrate at a stage where a circuit element and a wiring pattern are formed, or a semiconductor substrate at a stage where a circuit element is formed. Examples include substrates.
- a polishing apparatus that can be used in the polishing method of the present invention, for example, a holder that holds a substrate having a metal film to be polished and a polishing cloth (pad) can be attached, and a motor that can change the number of rotations.
- a general polishing apparatus having an attached polishing surface plate can be used.
- MIRRA manufactured by Applied Materials can be used.
- polishing cloth on the polishing surface plate there are no particular restrictions on general nonwoven fabrics and foamed polyurethanes. Or porous fluorine resin can be used.
- the polishing conditions are not particularly limited, but it is preferable to reduce the rotation speed of the surface plate to 200 rpm or less so that the substrate does not fly out.
- the polishing pressure of the substrate having the metal film to be polished on the polishing cloth is 5 to: LOOkPa, preferably from the viewpoint of uniformity in the surface of the metal film to be polished and the flatness of the pattern. It is preferable to be 0-50kPa! /.
- polishing may be performed by rotating or swinging the holder. Further, a polishing method in which a polishing surface plate is rotated on a planetary surface, a polishing method in which a belt-like polishing cloth is moved linearly in one direction in the longitudinal direction, and the like can be mentioned.
- the holder may be in a fixed, rotating, or swinging state.
- the metal polishing liquid to the polishing cloth with a pump or the like.
- the supply amount is not limited, but it is preferable that the surface of the polishing cloth is always covered with the polishing liquid. Specifically, it is preferable to supply 0.3 to 0.9 milliliter per lcm 2 of the polishing cloth area.
- the semiconductor substrate after polishing is thoroughly washed in running water and then force-dried by removing water droplets adhering to the semiconductor substrate using a spin dryer or the like.
- Hydrogen peroxide solution (special grade, 30% aqueous solution) 30% by weight, polishing agent weight, metal oxide solubilizers shown in Table 1, 0.4% by weight of benzotriazole, key-on functionality shown in Table 1
- a water-soluble polymer having a group of 0.4% by weight, and the remaining part was mixed with pure water so that the total amount would be 100% by weight, and the polishing liquids (A) to (F) of Examples 1 to 6 and Comparative Examples 1 to 2 Polishing liquids (I) to (J) were prepared.
- the pH of the polishing liquid was adjusted to the value shown in Table 1 depending on the amount of metal oxide solubilizer added. Arranged.
- Hydrogen peroxide solution (special grade, 30% aqueous solution) 30% by weight, polishing agent weight, metal oxide solubilizers shown in Table 1, 0.4% by weight of benzotriazole, key-on functionality shown in Table 1.
- the water-soluble polymer having a base of 0.4% by weight, colloidal silica barrels having a median diameter of 60 nm, 0.05% by weight, and the remainder is blended with pure water so that the total amount is 100% by weight.
- the polishing liquids (G) to (H) and the polishing liquid (K) of Comparative Example 3 were prepared. The pH of the polishing liquid was adjusted to the value shown in Table 1 depending on the addition amount of the acid-metal solubilizer.
- Hydrogen peroxide solution (reagent grade, 30% aqueous solution) 30% by weight, metal oxide solubilizer shown in Table 1, 0.4% by weight of benzotriazole, and 100% by weight in total. Pure water was added to the part to prepare a polishing liquid (L) of Comparative Example 4. The pH of the polishing liquid was adjusted to the value shown in Table 1 depending on the amount of the metal oxide solubilizer added.
- Hydrogen peroxide solution (special grade, 30% aqueous solution) 30% by weight with respect to the polishing liquid weight, metal oxide solubilizer shown in Table 1, 0.4% by weight of benzotriazole, water-soluble polymer (power) Polylysine, which is a thione polymer) 0.4% by weight, and the balance was mixed with pure water so that the total amount was 100% by weight.
- the pH of the polishing liquid was adjusted to the value shown in Table 1 depending on the amount of metal oxide solubilizer added.
- Hydrogen peroxide solution (special grade, 30% aqueous solution) 30% by weight with respect to the polishing liquid weight, metal oxide solubilizers shown in Table 1, 0.4% by weight of benzotriazole, and water-soluble polymers shown in Table 1.
- the remaining part was mixed with pure water so that the total amount was 4% by weight, and the polishing liquid (N) of Comparative Example 6 was prepared.
- the pH of the polishing liquid was adjusted to the value shown in Table 1 depending on the addition amount of the acidic metal solubilizer.
- No-turn silicon substrate A silicon dioxide insulating film layer is formed on the surface of the silicon substrate, a 15 nm TaN film, a 1 Onm Ta film, and a 1 OOnm copper film are formed by sputtering. We used a substrate to be polished on which 1.3 m of copper was deposited by the debonding method.
- Silicon substrate with no-turn After forming a silicon dioxide insulating film layer on the silicon substrate surface and forming a wiring groove in the silicon dioxide insulating film layer with a SEMATECH854 mask pattern, a sputtering method Then, a 15 nm TaN film, lOnm Ta film, and lOOnm copper film were formed, and a substrate to be polished on which 1.:m copper was deposited by electrolytic plating was used.
- the wiring groove depth is 500 mm.
- polishing device MIRRA manufactured by Applied Materials
- Copper polishing rate While supplying each of the polishing liquids (A) to (N) prepared above onto a polishing cloth, the silicon substrate without pattern was polished for 60 seconds under the above polishing conditions. The difference in copper film thickness before and after polishing was calculated from the electrical resistance value. The results are shown in Table 1.
- Dishing amount The silicon substrate with the above pattern was polished under the above polishing conditions while supplying each of the polishing liquids (A) to (N) prepared above onto a polishing cloth. The polishing was performed for 30 seconds with the force on the wafer and the excess copper completely removed, and the force was over-polished (additional polishing). Using a contact-type step meter (DECKTAK V200—Si manufactured by Veeco), the amount of reduction of the wiring metal part relative to the insulating film part was determined. The results are shown in Table 1.
- polishing flaws were confirmed by visual inspection, optical microscope observation, and electron microscope observation of the substrate after CMP treatment. As a result, in all of the examples and comparative examples, no significant polishing scratches were observed.
- the polishing liquid (I) of Comparative Example 1 having a pH of 3.5 is the polishing liquid (A) of Example 1 having a pH of 2.2 or the polishing liquid having a pH of 2.7. It can be seen that the amount of dishing is larger than the polishing liquid (B) in Example 2.
- the polishing liquid (J) of Comparative Example 2 having a pH of 3.5 is the polishing liquid (C) of Example 3 having a pH of 2.2 or the polishing liquid of Example 2 having a pH of 2.7. It can be seen that the amount of dating is larger than (D).
- the polishing liquid (K) of Comparative Example 3 in which the weight average molecular weight of the water-soluble polymer is as small as 7000 is the polishing liquid (G) of Example 7 or the polishing liquid of Example (8) in which the weight average molecular weight of the water-soluble polymer is large. It can be seen that the polishing rate is low and the dishing amount is large compared to liquid (H). It can also be seen that the polishing solution (L) of Comparative Example 4 having a pH of 2.2 and no water-soluble polymer has a low polishing rate and a large dishing amount. Further, it can be seen that the polishing liquid (M) of Comparative Example 5 using a cationic polymer has a low polishing rate and a large dishing amount. It can also be seen that the polishing liquid (N) of Comparative Example 6 having a small weight average molecular weight of the water-soluble polymer of 7000 has a low polishing rate and a large dishing amount.
- polishing liquids (A) to (H) of Examples 1 to 8 have a high polishing rate and a small amount of dating.
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- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
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- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
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Abstract
Description
Claims
Priority Applications (4)
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JP2007552965A JP4952584B2 (ja) | 2005-12-27 | 2006-12-27 | 金属用研磨液及び被研磨膜の研磨方法 |
US12/159,419 US8791019B2 (en) | 2005-12-27 | 2006-12-27 | Metal polishing slurry and method of polishing a film to be polished |
KR1020117006918A KR101260597B1 (ko) | 2005-12-27 | 2006-12-27 | 금속용 연마액 및 피연마막의 연마 방법 |
CN2006800494170A CN101346806B (zh) | 2005-12-27 | 2006-12-27 | 金属用研磨液以及被研磨膜的研磨方法 |
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JP (2) | JP4952584B2 (ja) |
KR (2) | KR101260597B1 (ja) |
CN (1) | CN101346806B (ja) |
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CN114213978A (zh) * | 2021-12-23 | 2022-03-22 | 广东欣科兴五金制品有限公司 | 一种铜合金表面抛光液及其制备方法 |
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KR101260597B1 (ko) | 2013-05-06 |
JPWO2007077886A1 (ja) | 2009-06-11 |
KR20110048563A (ko) | 2011-05-11 |
CN101346806A (zh) | 2009-01-14 |
US8791019B2 (en) | 2014-07-29 |
JP2012119697A (ja) | 2012-06-21 |
TWI343945B (en) | 2011-06-21 |
US20100178765A1 (en) | 2010-07-15 |
KR20080070074A (ko) | 2008-07-29 |
CN101346806B (zh) | 2010-09-29 |
TW200730614A (en) | 2007-08-16 |
JP4952584B2 (ja) | 2012-06-13 |
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