WO2003094216A1 - Fluide de polissage et procede de polissage - Google Patents
Fluide de polissage et procede de polissage Download PDFInfo
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- WO2003094216A1 WO2003094216A1 PCT/JP2003/005465 JP0305465W WO03094216A1 WO 2003094216 A1 WO2003094216 A1 WO 2003094216A1 JP 0305465 W JP0305465 W JP 0305465W WO 03094216 A1 WO03094216 A1 WO 03094216A1
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- Prior art keywords
- acid
- polishing
- group
- polishing liquid
- skeleton
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Classifications
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- 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
- B24B37/005—Control means for lapping machines or devices
- B24B37/0056—Control means for lapping machines or devices taking regard of the pH-value of lapping agents
-
- 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
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
- B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
- B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
-
- 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
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/04—Aqueous dispersions
-
- 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
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
- C23F3/06—Heavy metals with acidic solutions
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- 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 at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System 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]
Definitions
- the present invention relates to a polishing liquid, particularly a polishing liquid used in a wiring forming step of a semiconductor device, and a polishing method using the polishing liquid.
- LSI semiconductor integrated circuits
- CMP chemical mechanical polishing
- a common method of metal CMP is to attach a polishing pad (pad) on a circular polishing platen (platen), immerse the polishing pad surface with a polishing solution, and clean the surface of the base metal film. Press and apply the specified pressure from the back.
- the polishing platen is rotated while a force (polishing pressure or polishing load) is applied, and the metal film on the convex portion is removed by mechanical friction between the polishing liquid and the convex portion of the metal film.
- the polishing liquid used for CMP is generally composed of an oxidizing agent and solid abrasive grains, and a metal oxide dissolving agent and a metal anticorrosive are added as necessary. It is considered that the basic mechanism is to first oxidize the surface of the metal film by oxidation and then remove the oxide layer with solid abrasive grains. The oxide layer on the metal surface of the recesses does not touch the polishing cloth much and does not have the effect of shaving with solid abrasive grains.As the CMP progresses, the metal layer on the protrusions is removed and the substrate surface is flattened. Is done. Details of this are disclosed in the Journal of Electrochemical Society (Journal of the Electrochemical Society), Vol. 1, No. 38, 11 (issued in 1991), pp. 340-60-34464. Have been.
- conventional buried wiring formation by CMP involves the following problems: (1) the phenomenon that the central part of the surface of buried metal wiring is isotropically corroded and pitted like a dish (dating) and the wiring density Insulation film is also polished in the high part of the wiring, causing the metal wiring to become thinner (erosion or thinning); (2) polishing scratches (scratch); and (3) polishing of the substrate surface after polishing.
- the cleaning process for removing the remaining polishing residue is complicated, (4) the cost is increased due to the waste liquid treatment, and (5) the metal is corroded.
- Dishing ⁇ In order to suppress the corrosion of copper alloy during polishing and to form highly reliable LSI wiring, a metal oxide dissolving agent consisting of aminoacetic acid such as glycine or amide sulfuric acid and BTA (benzotoxin) are used. A method using a polishing liquid containing lyazol) has been proposed. This technique is described in, for example, Japanese Patent Application Laid-Open No. 8-83780.
- the pH of the polishing solution is set to be larger than (pKa-0.5).
- This technique is described in, for example, Japanese Patent No. 2819196.
- under the wiring such as copper or copper alloy, tantalum, titanium, titanium stainless steel, titanium nitride, and titanium nitride are used as barrier layers to prevent copper diffusion into the interlayer insulating film.
- tungsten nitride and a tantalum alloy, a titanium alloy, a tungsten alloy and other tantalum compounds, a titanium compound, a tungsten compound, and the like are formed.
- the exposed barrier layer must be removed by CMP.
- these conductor conductor films are harder than copper or copper alloys, so that a combination of polishing materials for copper or copper alloys cannot provide a sufficient CMP speed, and thus, the copper layer or copper alloy cannot be used.
- dishing occurs in copper or copper alloy and the wiring thickness is reduced. Therefore, a two-step polishing method comprising a first step of polishing copper or a copper alloy and a second step of polishing a Nori layer conductor is being studied.
- a high polishing rate can be obtained by adding a metal oxide dissolving agent to make the pH acidic, but in an acidic region, a high polishing rate can be obtained. Corrosion of copper alloy wiring easily occurs. Therefore, it was necessary to increase the concentration of the anticorrosive in the polishing liquid, to reduce the concentration of the metal oxide dissolving agent in the polishing liquid, or to use an acid having a low pKa and a low corrosiveness.
- polishing solution for polishing copper or copper alloy As a polishing solution for polishing copper or copper alloy, a high polishing rate is obtained. If an acid with a low pK a is used to increase the concentration of the metal oxide dissolving agent, or if the concentration of the anticorrosive is increased to suppress the etching rate, the polishing friction coefficient during polishing (dynamic friction coefficient) The metal wiring and its laminated film structure may be peeled off or disconnected, or the temperature rise due to friction may increase the chemical etching effect of the polishing liquid and increase the metal wiring. There was a problem that the dishing increased due to the corrosion of the steel.
- the present invention provides a polishing liquid and a polishing liquid which have high productivity, low dishing and erosion because the metal polishing rate is high, the etching rate is low, and the friction during polishing is low.
- An object of the present invention is to provide a polishing method using a polishing liquid. Further, according to the present invention, a highly reliable semiconductor device having excellent miniaturization, thinning, dimensional accuracy, and electrical characteristics can be provided. Disclosure of the invention
- the polishing liquid of the present invention relates to the following polishing liquid and polishing method.
- the metal oxide dissolving agent is an acid whose dissociation constant (PKa) of the first dissociable acidic group other than lactic acid, phthalic acid, fumaric acid, maleic acid and aminoacetic acid is less than 3.7
- One or more selected acids Group A), one or more selected from an ammonium salt of the Group A acid and an ester of the Group A acid; At least one acid selected from lactic acid, fumaric acid, fumaric acid, maleic acid, aminoacetic acid and acids having a pKa of the first dissociable acidic group of 3.7 or more
- the metal anticorrosive is at least one member selected from the group consisting of aromatic compounds having a triazole skeleton (Group C), an aliphatic compound having a triazole skeleton, and pyrimidine; At least one selected from the group consisting of a compound having a skeleton, a compound having an imidazole skeleton, a compound having a guanidine skeleton, a compound having a thiazole skeleton, and a compound having a pyrazole skeleton (Group D).
- a polishing liquid characterized by the following.
- the group A is composed of malonic acid, cunic acid, lingoic acid, glycolic acid, glutamic acid, dalconic acid, oxalic acid, tartaric acid, picolinic acid, nicotinic acid, mandelic acid, acetic acid, Consisting of sulfuric, nitric, phosphoric, hydrochloric and formic acids,
- the group B is composed of succinic acid, adipic acid, daltaric acid, benzoic acid, quinaldic acid, butyric acid, valeric acid, lactic acid, phthalic acid, fumaric acid, maleic acid and amino acetic acid. Polishing liquid.
- the metal oxide dissolving agent contains a combination of acids selected from the following, or a combination of at least one of which is an ammonium salt of an acid. Polishing liquid according to any one of (1) to (3):
- the metal anticorrosive has a triazole skeleton, a pyrimidine skeleton, a compound having an imidazole skeleton, a compound having a guanidine skeleton, or a compound having a thiazole skeleton.
- the polishing liquid according to any one of (1), (3) and (4), comprising at least one selected from a compound and a compound having a pyrazole skeleton.
- the aliphatic compound having a triazole skeleton of the group D is 1,2,3-triazole, 1,2,4-triazole, 3-7 minole 1 H—1,2,4—triazole and 41 amino 4H—1,2,4—at least one selected from triazole
- the compound having a pyrimidine skeleton is 4-aminopyrazo [3,4-d] pyrimidine, 1,2,4-triazolo [1,5-a] pyrimidine.
- the compound having an imidazole skeleton is 2 -methylimidazole, 2 -ethylimidazole, 2-(isopropyl) imidazole, 2 -propylimidazole, 2-butylimidazole.
- 4-methylimidazole, 2,4-dimethylimidazole, 21-ethyl-4-methylimidazole is at least one selected from (2), (5) to (8) The polishing liquid according to any one of the above.
- the pH is 3 to 4.5, and the concentration of the metal anticorrosive in the polishing solution is 0.01 to 0.5% by weight (1) to (10).
- the metal oxidizing agent is selected from hydrogen peroxide, ammonium persulfate, ferric nitrate, nitric acid, potassium periodate, hypochlorous acid, and ozonated water.
- the polishing liquid according to any one of (1) to (11), which is one of the above.
- the water-soluble polymer having a weight average molecular weight of 500 or more is polysaccharide, polycarboxylic acid, ester of polycarboxylic acid, salt of polycarboxylic acid, polyacrylamide, or vinyl polymer.
- a substrate is coated while supplying any of the polishing liquids (1) to (15) of the present invention on a polishing cloth of a polishing platen.
- the present invention relates to a polishing method characterized in that a polishing surface is polished by relatively moving a polishing cloth and a base while a polishing surface is pressed against the polishing cloth.
- the polishing method according to the second aspect of the present invention includes:-an inter-layer insulating film having a surface including a concave portion and a convex portion; a barrier layer covering the interlayer insulating film along the surface; A first polishing step of polishing a metal layer of a substrate having a metal layer covering the lower layer to expose the barrier layer of the convex portion; and at least a barrier after the first polishing step. A second polishing step of polishing the layer and the metal layer of the concave portion to expose the interlayer insulating film of the convex portion, wherein at least one of the first polishing step and the second polishing step is the polishing liquid of the present invention.
- the present invention relates to a polishing method for polishing using any one of (1) to (15).
- the metal layer preferably contains at least one selected from copper, a copper alloy, an oxide of copper, and an oxide of a copper alloy.
- the noria layer has a single-layer structure composed of one kind of composition or a laminated structure composed of two or more kinds of compositions, and the composition of the noria layer is made of tantalum, tantalum nitride, or tantalum. Alloys, other tantalum compounds, titanium, titanium nitride, titanium alloys, other titanium compounds, tungsten, tungsten nitride, tungsten alloys, and other tungsten compounds Is preferred. BRIEF DESCRIPTION OF THE FIGURES
- FIG. 1 is a schematic top view of an example in which a movable carrier / holder apparatus is mounted on a wafer polishing apparatus, wherein 1 is a carrier / holder apparatus, 2 is a polishing platen, and 3 is a polishing platen.
- the carrier, 4 is a roller, and 5 is a piezoelectric element.
- FIG. 2 is a schematic cross-sectional view showing an example of a state in which a wafer is polished by the wafer polishing apparatus shown in FIG. 1, in which 6 is a polishing cloth, 7 is a weight, 8 Is a pressure output meter, 9 is a carrier and holder support, 10 is a wafer, and 11 is a packing film with guides.
- 6 is a polishing cloth
- 7 is a weight
- 8 Is a pressure output meter
- 9 is a carrier and holder support
- 10 is a wafer
- 11 is a packing film with guides.
- the polishing liquid of the present invention contains (a) an oxidizing agent, (a) a metal oxide dissolving agent, (c) a metal anticorrosive, and water as main components.
- the oxidizing agent may be a metal oxide such as hydrogen peroxide, ammonium persulfate, ferric nitrate, nitric acid, potassium periodate, hypochlorous acid, and ozone water.
- Agents, of which hydrogen peroxide is particularly preferred. can be used alone or in combination of two or more.
- the substrate having a surface to be polished to which the polishing liquid is to be applied is a silicon substrate including an element for an integrated circuit, contamination by an alkali metal, an alkaline earth metal, a halogenated compound, etc. Oxidants that do not contain non-volatile components are desirable because they are not desirable. However, the composition of ozone water changes drastically with time, so hydrogen peroxide is most suitable.
- an oxidizing agent containing a nonvolatile component may be used.
- Examples of the (mouth) metal oxide dissolving agent in the present invention include the following acids, ammonium salts of the acids and esters of the acids, and are not particularly limited as long as they are water-soluble.
- Examples of the acid include malonic acid, cunic acid, lingoic acid, glutamic acid, dalconic acid, glycolic acid, succinic acid, lactic acid, adipic acid, glutaric acid, benzoic acid, and phthalic acid.
- Fumaric acid maleic acid, amino acid, oxalic acid, tartaric acid, picolinic acid, nicotinic acid, mandelic acid, acetic acid, sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, formic acid, quinaldic acid, butyric acid, valeric acid , Salicylic acid, glyceric acid, Pimelic acid and the like.
- the acids having a dissociation constant (p Ka) of the first dissociable acidic group of less than 3.7 among the acids having a dissociation constant (p Ka) of the first dissociable acidic group of less than 3.7, lactic acid, fumaric acid, fumaric acid, and maleic acid
- p Ka dissociation constant
- the compound selected from the Group A acid, the ammonium salt of the Group A acid, and the ester of the Group A acid is hereinafter referred to as Compound A.
- group B an acid having a pKa of the first dissociable acidic group of 3.7 or more, lactic acid (pKa: 3.66), and phthalic acid (pKa: 2.75) ), Fumaric acid (pKa: 2.85), maleic acid (pKa: 1.75) and aminoacetic acid (pKa: 2.36)
- group B an acid having a pKa of the first dissociable acidic group of 3.7 or more, lactic acid (pKa: 3.66), and phthalic acid (pKa: 2.75) ), Fumaric acid (pKa: 2.85), maleic acid (pKa: 1.75) and amino
- the dissociation constant (p Ka) of the first dissociable acidic group of lactic acid, phthalic acid, fumaric acid, maleic acid and aminoacetic acid is less than 3.7, but the etching effect on metals is relatively low. Classified into group B because it is very small.
- the metal anticorrosive includes a compound having a triazole skeleton, a compound having a pyrimidine skeleton, a compound having an imidazole skeleton, a compound having a guanidine skeleton, and a compound having a thiazole skeleton And compounds having a pyrazole skeleton, and the like, and are not particularly limited.
- a group of aromatic compounds having a triazole skeleton as a metal anticorrosive is hereinafter referred to as Group C, and an aliphatic compound having a triazole skeleton;
- a compound having a pyridine skeleton, a compound having an imidazole skeleton, a compound having a guanidine skeleton, a compound having a thiazole skeleton, and a compound having a pyrazole skeleton The group of compounds that perform this is hereinafter referred to as Group D.
- the polishing liquid of the present invention comprises (mouth) one or more of the above compound A and one or more of the above compound B as a metal oxide dissolving agent,
- a polishing liquid that satisfies at least one of at least one selected from the above group C and one or more selected from the above group D as a metal anticorrosive.
- acids included in the above-mentioned group A include malonic acid, citric acid, lingoic acid, glycolic acid, glutamic acid, dalconic acid, oxalic acid, tartaric acid, picolinic acid Acid, nicotinic acid, mandelic acid, acetic acid, sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, formic acid and the like.
- acids contained in the above group B include succinic acid, adipic acid, daltaric acid, benzoic acid, quinaldic acid, butyric acid, valeric acid, lactic acid, phthalic acid, fumaric acid, maleic acid, and aminic acid Examples thereof include acetic acid, salicylic acid, dali seric acid, and pimelic acid.
- Esters formed by acids of Group A or Group B include methyl ester, ethyl ester, 1-propyl ester, 2-propyl ester, 1-butyl ester, 2-butyl ester, 3-butyl ester, t-butyl ester, etc. And methyl ester, ethyl ester, 1-propyl ester, and 2-propyl ester.
- Compound A may contain two or more different acids within Group A. Also, two or all three of acids, ammonium salts, and esters And in that case, each of the acid, ammonium salt and ester may use a different acid in Group A. The same applies to compound B.
- the acids in Group A are malonic acid, citric acid, lingoic acid, glycolic acid, and glutamate.
- the acid of group B is succinic acid, It is preferably composed of adipic acid, daltaric acid, benzoic acid, quinaldic acid, butyric acid, valeric acid, lactic acid, phthalic acid, fumarylic acid, maleic acid and aminoacetic acid.
- the metal oxide dissolving agent is one of the following combinations of Group A and Group B. It is preferable to include compound A and compound B described above.
- the (mouth) metal oxide solubilizer comprises an acid combination selected from the following combinations, or at least one of the combinations selected from the following is an ammonium salt of an acid. Includes certain combinations.
- the ratio of compound A to compound B contained in the metal oxide dissolving agent may be such that the effect of the present invention is not impaired, but is preferably 5: 1 to 1:10 by weight ratio, and 2: 2! To 1: 3 is more preferred, and 1: 1 to 1: 2 is particularly preferred.
- Aromatic compounds having a triazole skeleton of Group C include benzotriazole, 1-hydroxybenzotriazole, 1-dihydroxypropylbenzotriazole, and 2,3- Dicarboxypip Pirvenzotriazole, 4—Hydroxybenzotriazole, 4Holepoxyl (1-1H_) Benzotriazole, 41carboxyl (1-1H—) Benzotriazole methyl ester, 4-force lipoxyl (1-1H—) benzotriazole butyl ester, 4-carboxyl (1-1H_) benzotriazole octyl ester, 5-hexylbenzoto Razolyl, [1,2,3—benzotriazolyl-1-methyl] [1,2,4, triazolyl 1-methyl] [2—ethylhexyl ] Amin, Tril Triazo Naphthoquinone harvest Re ⁇ zone Ichiru, bis [(1 one benzo Application Benefits Azori) methyl] phospho phosphat
- the group C is composed of benzotriazole, 1-hydroxybenzotriazole and 5-methylbenzotriazole in terms of polishing rate and etching rate.
- Metallic anticorrosives can be selected from these group C alone or in combination of two or more. It is.
- the aliphatic compounds having a triazole skeleton include 1,2,3—triazole, 1,2,4-triazole, and 3-7 minor.
- 1 H — 1, 2, 4 — Triazole, 3 — Amino triazole, 4 — Amino 4 H — 1, 2, 4, 4-triazole, etc. Is exemplified.
- 1,2,3—triazole, 1,2,4—triazole, and 3—amino 1 H-1,2,4—triazole Preferably, it is selected from zole and 4-amino-4H-1,2,4-triazole. These compounds can be selected alone or in combination of two or more.
- Examples of the compound having an imidazole skeleton include 2-methylimidazole, 2-ethylethylimidazole, 2_ (isopropyl) imidazole, and 2-propylimidazole, 2—Butylimidazole, 4-Methylimidazole, 2,4—Dimethylimidazole, 21-Ethyl—4—Methylimidazole, 2—Indecylimidazole, 2—Aminoimidazole Etc. can be exemplified.
- it is selected from dazole, 4-methylimidazole, 2,4-dimethylimidazole and 2-ethyl-4-methylimidazole.
- One of these compounds can be selected alone, or two or more of them can be selected in combination.
- Compounds having a pyrimidine skeleton include pyrimidine, '1,2,4_triazo-mouth [1,5-a] pyrimidine, 1,3,4,6,7 , 8-hexahydrid mouth -2H-pyrimido [1, -a] pyrimidine, 1,3-diphenyl-pyrimidine -2,4,6-trion, 1,, 5, 6-tetrahydrid pyrimidine, 2, 4, 5, 6- Tetraaminopyrimidine sulfate, 2,4,5-trino, hydroxypyrimidine, 2,4,6-triaminopyrimidine, 2,4 , 6-Tricyclopyrimidine, 2,4,6-Trimethoxypyrimidine, 2,4,6-Triphenylpyrimidine, 2,4-Diamino -6-Hydroxyl pyrimidine, 2,4-Diaminopyrimidine, 2-Acetamide pyrimidine, 2-Aminopyrimidine, 2- Methyl-5,7-diphenyl- (1,2,4)
- Examples of the compound having a guanidine skeleton include 1,3-diphenyldanidine, 1-methyl-3-12-troguanidine, and the like.
- Examples of the compound having a thiazole skeleton include 2-mercaptobenzothiazole. Each of these compounds can be selected alone or in combination of two or more.
- the metal anticorrosives as Group D are selected from the above compounds by one kind alone or in combination of two or more kinds.
- the ratio of the compound selected from the group C and the compound selected from the group D contained in the metal anticorrosive may be such that the effect of the present invention is not impaired, but is 10: 1 to 1: 1 by weight. 10 is preferred, 5: 1 to 1: 7.5 is more preferred, and 3: 1 to 1: 6 is particularly preferred.
- the pH of the polishing liquid must be between 2 and 5, preferably between 3 and 4.5, and more preferably between 3.5 and 4.3. If the pH is less than 2, problems such as metal corrosion and surface roughness are likely to occur, and the concentration of the metal anticorrosive is increased in order to reduce the problem, and the polishing friction coefficient is also reduced. It becomes large, and wiring failure is likely to occur. On the other hand, if the pH is greater than 5, the corrosion effect of the metal is small, so that the concentration of the metal anticorrosive can be reduced, but it is difficult to obtain a sufficient polishing rate.
- the pH of the polishing liquid of the present invention can be adjusted by the amount of acid added. It can also be adjusted by adding an alkali component such as ammonia, sodium hydroxide, tetramethylammonium hydroxide mouth oxide (TMAH).
- TMAH tetramethylammonium hydroxide mouth oxide
- the pH of the polishing liquid of the present invention was measured with a pH meter (for example, Mode IP 81 of Yokogawa Electric Corporation).
- Use standard buffer phthalate pH buffer: 4.21 (25 ° C), neutral phosphate buffer: pH 6.86 (25 ° C)
- the electrodes were placed in the polishing solution, and the values were measured after two minutes had passed and stabilized.
- the polishing liquid of the present invention may contain a water-soluble polymer for improving dishing and erosion of metal wiring.
- the water-soluble polymer is not particularly limited, and preferably has a weight average molecular weight of 500 or more.
- Polysaccharides such as, for example, alginic acid, pectic acid, carboxymethylcellulose, agar, rihdran and pullulan;
- Polyaspartic acid Polyglutamic acid, Polylysine, Polylingic acid, Polymethacrylic acid, Polyamide acid, Polymaleic acid, Polytako Acid, polyfumaric acid, poly (p-styrenecarbonic acid), polyacrylic acid, polyamide acid, and polycarboxylic acid such as polyoxylic acid;
- Vinyl polymers such as polyvinyl alcohol, polyvinylpyrrolidone, and polyacrylene
- polysaccharides polycarboxylic acids, esters of polycarboxylic acids, salts of polycarboxylic acids, polyacrylamides, and vinyl polymers are preferred.
- pectic acid agar
- Poly lactic acid
- poly (vinyl alcohol) and poly (vinyl alcohol) their esters and their ammonium salts are preferred.
- the substrate to be applied is a silicon substrate for semiconductor integrated circuits, etc.
- contamination with alkali metals, alkaline earth metals, halides, etc. is not desirable.
- Salt is preferred. If the substrate is a glass substrate or the like, this is not always the case.
- the compounding amount of the oxidizing agent in the present invention is preferably 0.01 to 50 g, more preferably 0.1 to 30 g, based on 100 g of the total amount of the polishing liquid. However, it is particularly preferable that the weight be 0.2 to 15 g. When the amount is less than 0.01 g, the metal tends to be insufficiently oxidized and the CMP rate tends to be low. On the other hand, when the amount exceeds 50 g, a thick oxide film layer is formed on the metal surface and the polishing rate is reduced. Tends to decrease.
- the mixing amount of the metal oxide dissolving agent component in the present invention is preferably 0.01 to 1 Og, and more preferably 0.01 to 1 lg, based on 100 g of the total amount of the polishing liquid. More preferably, it is particularly preferably from 0.01 to 0.5 g. If this amount is less than 0.001 g The polishing rate tends to decrease. If the polishing rate exceeds 10 g, the etching rate increases, the corrosion of metal wiring becomes a problem, and if the addition amount of the metal anticorrosive is increased to suppress the etching rate, Abrasion friction tends to increase.
- the amount of the metal anticorrosive in the present invention is preferably 0.001 to 2.0 g with respect to 100 g of the polishing liquid. That is, it is preferable that the amount is 0.01 to 2.0% by weight, more preferably 0.01 to 0.5% by weight, based on the total weight of the polishing liquid. It is particularly preferred that the content be 0.02 to 0.15% by weight. If the amount is less than 0.001% by weight, the suppression of etching tends to be difficult. If the amount exceeds 2.0% by weight, a practical polishing rate tends not to be obtained.
- the amount of the water-soluble polymer is preferably 0.001 to 10 g per 100 g of the polishing liquid. , And more preferably 0.1 to 1 g, and particularly preferably 0.1 to 1 g. If the amount is less than 0.001 g, dishing of metal wiring deteriorates, and the accumulation of objects to be polished on the polishing cloth tends to increase. Therefore, it tends to be difficult to achieve both polishing speed and in-plane uniformity.
- the weight-average molecular weight of the water-soluble polymer is preferably at least 500, more preferably at least 5,000, more preferably at least 10,000. Is particularly preferred.
- the upper limit of the weight average molecular weight is not particularly specified, but is not more than 500,000 from the viewpoint of solubility. If the weight average molecular weight is less than 50,000, a high polishing rate tends not to be exhibited. In the present invention, it is preferable to use at least one or more water-soluble polymers having a weight average molecular weight of 500 or more.
- the polishing liquid of the present invention includes, in addition to the above-described materials, abrasive grains such as alumina, silica, and cerium, surfactants, dyes such as Victory Pure, and phthalocyanine. Coloring agents such as pigments and the like may be included.
- an organic solvent may be contained, and the organic solvent is preferably one that can be arbitrarily mixed with water.
- the organic solvent is preferably one that can be arbitrarily mixed with water.
- methanol, ethanol, 2-propanol, tetrahydrofuran, ethylene glycol, acetate, methylethylketone and the like can be mentioned.
- the abrasives include inorganic abrasives such as silica, alumina, zirconia, celia, titania, and silicon carbide; and organic materials such as polystyrene, polyacryl, and polyvinyl chloride.
- Abrasive grains may be used, but solid abrasive grains selected from one or more of alumina, silica and cerium are preferred. Further, the dispersion stability in the polishing solution is good, the number of polishing scratches (scratch) generated by CMP is small, and the average particle diameter is 100 nm or less.
- colloidal aluminum are preferred, and the average particle size is 80 nm or less. Colloidal aluminum is more preferred, and the average particle size is 60 nm or less.
- Mosquitoes are most preferred.
- colloidal silicide a production method by hydrolysis of silicon alkoxide or ion exchange of sodium silicate is known, and colloidal alumina is made of aluminum nitrate.
- a production method by hydrolysis is known.
- the particle size of the abrasive grains in the present invention was measured by a light diffraction scattering type particle size distribution meter (for example, model number COULTER N SD manufactured by COULTER Electronics).
- the degree of aggregation of the particles was measured with a transmission electron microscope (for example, model number H-7100FA manufactured by Hitachi, Ltd.).
- the measurement conditions of the particle size distribution meter are as follows: measurement temperature 20 ° C, solvent refractive index 1.33 (water), particle refractive index Unknown (setting), solvent viscosity 1.005 cp (water), Run Time 200 seconds, laser incident angle 90 °, and Intensity (corresponding to scattering intensity and turbidity) are in the range of 5E + 04 to 4E + 05 Thus, when it was higher than 4E + 05, it was diluted with water and measured.
- the concentration of the abrasive grains is preferably from 0.01 to 10.0% by weight, more preferably from 0.05 to 2.0% by weight, based on the total weight of the polishing liquid. 0.1 to 1.0% by weight is most preferred. If the abrasive grain concentration is less than 0.01% by weight, there is no effect of adding the abrasive grains, and there is no difference in the effect even if it is added more than 10.0% by weight.
- the polishing cloth and the substrate are pressed while the polishing surface of the substrate is pressed against the polishing cloth while supplying the polishing liquid of the present invention onto the polishing cloth of the polishing platen.
- This is a polishing method that relatively moves the surface to be polished.
- a substrate in the process of manufacturing a semiconductor device is preferably used.
- an interlayer insulating film having a surface formed of a concave portion and a convex portion, a norial layer covering the interlayer insulating film along the surface, and a barrier filled with the concave portion.
- Polishing a metal layer of a substrate having a metal layer covering the layer to expose the barrier layer of the convex portion hereinafter referred to as a first polishing step
- a first polishing step and a second polishing step in particular, a step of exposing the interlayer insulating film of the convex portion by polishing the metal layer of the concave portion and the concave portion. At least one of these is a polishing method for polishing using the polishing liquid of the present invention.
- the second polishing step can be polished with the polishing liquid of the present invention subsequent to the first polishing step.
- the insulating film of the interlayer insulating film include a silicon-based film and an organic polymer film.
- the silicon-based coating include organosilicate glass obtained from silicon dioxide, fluorosilicate glass, and trimethylsilanedimethoxydimethylsilane as a starting material. And silicon-based coatings such as silicon oxynitride and hydrogenated silsesquioxane, as well as silicon nitride and silicon nitride.
- organic polymer film a wholly aromatic low dielectric constant interlayer insulating film may be used.
- organosilicate glass is preferred. These films are formed by a CVD method, a spin coat method, a dip coat method, or a spray method.
- the barrier layer is formed to prevent metal such as copper from diffusing into the interlayer insulating film and to improve adhesion between the insulating film and the metal.
- the nori layer is made of tantalum, tantalum nitride, tantalum alloy, other tantalum compounds, titanium, titanium nitride, titanium alloy, other titanium compounds, tungsten, tungsten nitride, titanium nitride. It is preferable that at least one selected from the group consisting of tungsten alloys and other tungsten alloys is used, and that it has a single-layer structure composed of one composition or a composition composed of two or more compositions. It is preferable to have a laminated structure.
- the metal layer examples include a layer mainly containing a metal such as copper, a copper alloy, a copper oxide, a copper alloy oxide, tungsten, a tungsten alloy, silver, and gold. Of these, it is preferred to polish a layer containing at least one selected from copper, copper alloys, copper oxides and copper alloy oxides.
- the metal layer can be formed on the NOR layer by a known sputtering method or plating method.
- polishing for example, when polishing with a polishing cloth, a holder for holding a semiconductor substrate and a polishing cloth (polishing pad) are attached, and a mode in which the number of rotations can be changed is set. Polishing fixture with evening etc. A general polishing apparatus having a disk can be used.
- polishing cloth on the polishing platen general nonwoven fabric, foamed polyurethane, porous fluororesin and the like can be used, and there is no particular limitation. Also, it is preferable that the polishing cloth is subjected to groove processing such that the polishing liquid is retained.
- the polishing conditions are not limited, but the rotation speed of the platen is preferably as low as 200 rpm or less so that the substrate does not pop out.
- the pressing pressure (processing load) of the semiconductor substrate having the surface to be polished against the polishing cloth is preferably 1 kPa to 100 kPa, and the uniformity of the polishing rate within the wafer surface and In order to satisfy the flatness of the pattern, it is more preferable to be 5 kPa to 50 kPa.
- the polishing liquid of the present invention is continuously supplied to the polishing cloth by a pump or the like.
- the supply amount is not limited, but it is preferable that the surface of the polishing pad is always covered with the polishing liquid.
- the polishing surface is polished by moving the polishing cloth and the substrate relatively while the polishing surface is pressed against the polishing cloth while supplying the polishing liquid onto the polishing cloth on the polishing platen. can do.
- the holder may be rotated or rocked for polishing.
- a polishing method in which a polishing platen is rotated in a planetary manner, a polishing method in which a belt-shaped polishing cloth is linearly moved in one direction in a longitudinal direction, and the like are exemplified.
- the holder 1 may be in a fixed, rotating, or swinging state. These polishing methods can be appropriately selected depending on the surface to be polished and the polishing apparatus as long as the polishing cloth and the substrate are relatively moved.
- the semiconductor substrate is preferably washed well in running water, and then dried using a spin dryer or the like to remove water droplets attached to the semiconductor substrate.
- polishing method of the present invention will be described with reference to semiconductor devices. A description will be given along the formation of the wiring layer.
- an interlayer insulating film such as silicon dioxide is laminated on a silicon substrate.
- a concave portion substrate exposed portion having a predetermined pattern is formed on the surface of the interlayer insulating film to form an interlayer insulating film composed of a convex portion and a concave portion.
- a barrier layer such as tantalum covering the interlayer insulating film is formed along with the unevenness of the surface by vapor deposition or CVD.
- a metal layer such as copper for covering the barrier layer is formed by vapor deposition, plating, or CVD so as to fill the recess.
- the thicknesses of the interlayer insulating film, the norm layer and the metal layer are preferably about 0.01 to 2.0 Mm, 1 to: L0.0nm, and about 0.01 to 2.5 m, respectively.
- this semiconductor substrate is fixed to a polishing apparatus, and the metal layer on the surface is used as a surface to be polished, and polishing is performed while supplying the polishing liquid of the present invention.
- the desired conductor pattern is obtained in which the barrier layer at the convex portion of the interlayer insulating film is exposed on the substrate surface, and the metal layer is left in the concave portion of the interlayer insulating film.
- polishing liquid of the present invention is supplied by using the conductor pattern as a surface to be polished and at least the exposed metal layer of the barrier layer and the exposed barrier layer as a surface to be polished. While polishing. A desired pattern in which the interlayer insulating film below the barrier layer of the projection is entirely exposed, the metal layer serving as a wiring layer is left in the recess, and the cross section of the barrier layer is exposed at the boundary between the projection and the recess. The polishing is terminated when the value is obtained.
- polishing for example, if the time required to obtain the desired pattern in the second polishing step is 100 seconds, this Polishing for additional 50 seconds in addition to polishing for 100 seconds is referred to as overpolishing 50%.
- the polishing surface is polished by relatively moving the polishing cloth and the substrate while pressing the polishing surface of the substrate against the polishing cloth.
- a method in which a metal or resin brush is brought into contact, and a polishing method in which a polishing liquid is sprayed at a predetermined pressure are also used.
- the effects of the metal oxide dissolving agent and the metal anticorrosive in the polishing liquid are well balanced. Since the polishing rate of the surface to be polished is high and the etching rate is low without increasing the polishing friction coefficient, the advantage that the amount of dicing is small can be obtained.
- the etching rate is preferably 3 nm / min or less, more preferably 2 nmZ / min or less, and particularly preferably 1.5 nmZ / min or less.
- the polishing coefficient of friction is preferably 0.7 or less, more preferably 0.4 or less.
- polishing may be performed using the polishing liquid of the present invention.
- the polishing liquid of the present invention used in the first polishing step and the second polishing step may have the same composition or a different composition, but if the composition is the same, the polishing liquid does not stop from the first polishing step to the second polishing step. Excellent productivity because polishing can be continued continuously.
- an interlayer insulating film and a second-layer metal wiring are further formed, and an interlayer insulating film is formed again between the wirings and on the wiring, and then polished.
- the surface should be smooth over the entire surface of the semiconductor substrate.
- polishing solution weight Based on the polishing solution weight, (a) 25% by weight of hydrogen peroxide solution (special grade reagent, 30% aqueous solution) as an oxidizing agent, and (mouth) as a metal oxide dissolving agent are shown in Tables 1-2. (3) Benzotriazole (BTA) in the amounts shown in Tables 1-2 as metal anticorrosives, and water solubility with an average weight molecular weight of 200,000 Pure water was blended so that 0.4% by weight of polymer and 0.2% by weight of colloidal silica abrasive having an average particle diameter of 60 nm were added to make up a total of 100% by weight. Polishing liquids of Examples 1 to 6 and Comparative Examples 1 to 6 were prepared. The pH of the polishing solution was adjusted with aqueous ammonia (25%) so that the values shown in Tables 1-2 were obtained after mixing with pure water.
- Silicon substrate Silicon substrate Z Silicon dioxide film thickness 300 nm Z Barrier layer: Tantalum nitride film thickness 25 5 mZ Copper film thickness 1.2 m
- Polishing liquid supply rate 50 c c / min
- Polishing device Depth-weight experimental polishing device (polishing platen diameter: ⁇ 40 cm)
- Polishing cloth Polyurethane foam resin (Model: Ic 100, manufactured by Kuchi Dale) Polishing pressure: 21 kPa
- Etching rate The above two types of substrates were immersed in the above-mentioned agitated polishing liquid (room temperature, 25 ° C, agitation 100 rpm), and the difference in copper layer thickness before and after immersion was calculated from the electrical resistance value. Was. Approximately the same value was obtained from the two types of substrates, and the value of the substrate without a pattern was adopted.
- Polishing rate of copper by CMP The above two kinds of substrates were polished under the above polishing conditions while supplying each polishing liquid prepared above on a polishing cloth. The difference in Cii film thickness before and after polishing was calculated from the electrical resistance value. Approximately the same value was obtained from the two types of substrates, and the value of the substrate without a pattern was adopted.
- Dishing amount Silicon substrate as substrate, with wiring density of 50% After forming a groove with a wiring width of 0.35 to 1011 and a depth of 0.5_im, and then forming a silicon dioxide film with a thickness of 300 nm by a known plasma CVD method, A 50-nm-thick tantalum nitride film was formed as a barrier layer by the sputtering method described above, and a copper film was similarly formed to a thickness of 1.2 m by the sputtering method and embedded by a known heat treatment. did.
- the copper film was polished under the same conditions as the evaluation of the polishing rate until the tantalum nitride barrier layer was exposed on the entire surface of the substrate.
- the wiring metal width for the insulating film portion was determined from the surface shape of the stripe-shaped pattern portion in which the wiring metal portion width and the insulating film width were alternately arranged. The amount of film reduction in the part was determined.
- FIG. 1 is a schematic top view of an example of a wafer polishing apparatus equipped with a movable carrier / holder apparatus.
- FIG. 2 is a schematic cross-sectional view showing an example of a state in which a wafer is being polished by the wafer polishing apparatus shown in FIG.
- a 12.7 cm (5 inch) wafer polishing machine equipped with a movable carrier holder device 1 as shown in these figures was prepared.
- the carrier / holder unit 1 is supported by a carrier / holder column 9.
- a polishing cloth 6 is attached to the upper surface of the polishing platen 2 of the polishing apparatus.
- the polishing pressure is adjusted with a weight 7.
- the polishing liquid is supplied onto the polishing cloth from a polishing liquid supply device (not shown).
- the wafer 10 having no pattern among the above substrates was fixed to the lower part of the carrier 3 of the carrier holder device 1 by the packing film 11 with a guide, with the surface to be polished facing the polishing cloth. Polishing of the Cu film was started under the same conditions as the evaluation of the polishing rate above, and two minutes after the start of polishing, the force applied to the piezoelectric element 5 through the roller 14 of the carrier 'holder device 1' was changed by Kyowa Co., Ltd. An electric signal was read by a load converter (model number LM-50 KA) manufactured by Dengyo, and this value was converted into a frictional force by a pressure output meter 8 to calculate a polishing friction coefficient. Examples 1 to 8 and Comparative Example 1 Tables 1 to 3 also show the etching rates of No. 8 to 8, the polishing rate of copper by CMP, the dishing amount, and the polishing friction coefficient.
- Comparative Example 1 only the organic acid of Group A having a relatively small pKa was used alone as a metal oxide dissolving agent.In order to suppress the etching rate, the concentration of the metal anticorrosive benzotriazole was reduced. Because of the high amount, the dishing amount is large and the abrasive friction is large. In Comparative Example 3, since two kinds of acids having a pKa of Group A of less than 3.7 were used, the concentration of the anticorrosive was high, the amount of dicing was large, and the abrasive friction was large. In Comparative Examples 2 and 4 in which the amount of the metal anticorrosive was suppressed, the etching rate did not decrease to an appropriate range.
- Comparative Examples 7 and 8 only benzotriazole of Group C was used as the metal anticorrosive, and in Comparative Example 7, the concentration of the metal anticorrosive was increased to suppress the etching rate to a practical range. The amount of tsushing is large and the friction coefficient of polishing is large. In Comparative Example 8 in which the concentration of the metal anticorrosive was suppressed, the polishing coefficient of friction was small, but the etching rate was large, and the dishing amount did not decrease to the proper range. On the other hand, in Examples 7 and 8, etching was suppressed at a relatively low concentration of the metal anticorrosive agent, the polishing friction coefficient was small, and good dishing characteristics were obtained.
- the polishing rate of the metal is high, the etching rate is low, and the balance between the two is good. Therefore, the polishing friction is reduced at a low concentration of the metal anticorrosive, the productivity is high, and the dishing and erosion of the metal wiring are performed.
- a polishing liquid with a small portion can be obtained.
- the polishing method of the present invention using this polishing liquid is suitable for use in the manufacturing process of highly reliable semiconductor devices and various electronic component devices with excellent miniaturization, thinning, dimensional accuracy, electrical characteristics, and productivity. is there.
Description
Claims
Priority Applications (9)
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CNB038095904A CN100336179C (zh) | 2002-04-30 | 2003-04-28 | 研磨液及研磨方法 |
EP03719239A EP1505639B1 (en) | 2002-04-30 | 2003-04-28 | Polishing fluid and polishing method |
KR1020047017363A KR100720985B1 (ko) | 2002-04-30 | 2003-04-28 | 연마액 및 연마방법 |
AU2003235964A AU2003235964A1 (en) | 2002-04-30 | 2003-04-28 | Polishing fluid and polishing method |
DE60322695T DE60322695D1 (de) | 2002-04-30 | 2003-04-28 | Polierfluid und polierverfahren |
US10/513,002 US7367870B2 (en) | 2002-04-30 | 2003-04-28 | Polishing fluid and polishing method |
JP2004502340A JP4449745B2 (ja) | 2002-04-30 | 2003-04-28 | 研磨液及び研磨方法 |
US11/808,047 US8696929B2 (en) | 2002-04-30 | 2007-06-06 | Polishing slurry and polishing method |
US11/808,038 US20070295934A1 (en) | 2002-04-30 | 2007-06-06 | Polishing slurry and polishing method |
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JP2002128644 | 2002-04-30 | ||
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JP2002-160159 | 2002-05-31 |
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US11/808,038 Division US20070295934A1 (en) | 2002-04-30 | 2007-06-06 | Polishing slurry and polishing method |
US11/808,047 Division US8696929B2 (en) | 2002-04-30 | 2007-06-06 | Polishing slurry and polishing method |
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US (3) | US7367870B2 (ja) |
EP (2) | EP1881524B1 (ja) |
JP (2) | JP4449745B2 (ja) |
KR (1) | KR100720985B1 (ja) |
CN (2) | CN100336179C (ja) |
AT (2) | ATE470236T1 (ja) |
AU (1) | AU2003235964A1 (ja) |
DE (2) | DE60322695D1 (ja) |
TW (1) | TWI303660B (ja) |
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Also Published As
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CN101037585A (zh) | 2007-09-19 |
JP4853494B2 (ja) | 2012-01-11 |
ATE470236T1 (de) | 2010-06-15 |
JP4449745B2 (ja) | 2010-04-14 |
US20080003924A1 (en) | 2008-01-03 |
TWI303660B (en) | 2008-12-01 |
EP1881524A1 (en) | 2008-01-23 |
DE60332881D1 (de) | 2010-07-15 |
DE60322695D1 (de) | 2008-09-18 |
EP1505639A1 (en) | 2005-02-09 |
US7367870B2 (en) | 2008-05-06 |
AU2003235964A1 (en) | 2003-11-17 |
US20070295934A1 (en) | 2007-12-27 |
CN101037585B (zh) | 2010-05-26 |
CN100336179C (zh) | 2007-09-05 |
EP1505639A4 (en) | 2007-05-09 |
US20050181609A1 (en) | 2005-08-18 |
KR100720985B1 (ko) | 2007-05-22 |
US8696929B2 (en) | 2014-04-15 |
JP2008263215A (ja) | 2008-10-30 |
EP1881524B1 (en) | 2010-06-02 |
TW200307032A (en) | 2003-12-01 |
ATE403936T1 (de) | 2008-08-15 |
KR20050006203A (ko) | 2005-01-15 |
CN1650403A (zh) | 2005-08-03 |
JPWO2003094216A1 (ja) | 2005-09-08 |
EP1505639B1 (en) | 2008-08-06 |
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