WO2014119390A1 - 研磨パッド - Google Patents
研磨パッド Download PDFInfo
- Publication number
- WO2014119390A1 WO2014119390A1 PCT/JP2014/050820 JP2014050820W WO2014119390A1 WO 2014119390 A1 WO2014119390 A1 WO 2014119390A1 JP 2014050820 W JP2014050820 W JP 2014050820W WO 2014119390 A1 WO2014119390 A1 WO 2014119390A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- polishing
- polishing pad
- isocyanate
- weight
- prepolymer
- Prior art date
Links
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- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000011417 postcuring Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical compound CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000007261 regionalization Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- RUELTTOHQODFPA-UHFFFAOYSA-N toluene 2,6-diisocyanate Chemical compound CC1=C(N=C=O)C=CC=C1N=C=O RUELTTOHQODFPA-UHFFFAOYSA-N 0.000 description 1
- VOZKAJLKRJDJLL-UHFFFAOYSA-N tolylenediamine group Chemical group CC1=C(C=C(C=C1)N)N VOZKAJLKRJDJLL-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- 125000003258 trimethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])[*:1] 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/11—Lapping tools
- B24B37/20—Lapping pads for working plane surfaces
- B24B37/24—Lapping pads for working plane surfaces characterised by the composition or properties of the pad materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/341—Dicarboxylic acids, esters of polycarboxylic acids containing two carboxylic acid groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
- C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7614—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring
- C08G18/7621—Polyisocyanates or polyisothiocyanates cyclic aromatic containing only one aromatic ring being toluene diisocyanate including isomer mixtures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30625—With simultaneous mechanical treatment, e.g. mechanico-chemical polishing
Definitions
- the present invention stabilizes flattening processing of optical materials such as lenses and reflecting mirrors, silicon wafers, glass substrates for hard disks, aluminum substrates, and materials that require high surface flatness such as general metal polishing processing,
- the present invention relates to a polishing pad that can be performed with high polishing efficiency.
- the polishing pad of the present invention is particularly suitable for a step of planarizing a silicon wafer and a device having an oxide layer, a metal layer, etc. formed thereon, before further laminating and forming these oxide layers and metal layers. Used for.
- a typical material that requires a high degree of surface flatness is a single crystal silicon disk called a silicon wafer for manufacturing a semiconductor integrated circuit (IC, LSI).
- Silicon wafers have a highly accurate surface in each process of stacking and forming oxide layers and metal layers in order to form reliable semiconductor junctions of various thin films used for circuit formation in IC, LSI, and other manufacturing processes. It is required to finish flat.
- a polishing pad is generally fixed to a rotatable support disk called a platen, and a workpiece such as a semiconductor wafer is fixed to a polishing head.
- a polishing operation is performed by generating a relative speed between the platen and the polishing head by both movements, and continuously supplying a polishing slurry containing abrasive grains onto the polishing pad.
- the polishing characteristics of the polishing pad are required to be excellent in the flatness (planarity) and in-plane uniformity of the material to be polished and have a high polishing rate.
- the flatness and in-plane uniformity of the material to be polished can be improved to some extent by increasing the elastic modulus of the polishing layer.
- the polishing rate can be improved by increasing the amount of slurry retained by using a foam containing bubbles.
- Patent Document 1 discloses a polishing cloth used for flattening a material to be flattened having a level difference, and a polishing surface has a portion having a partially different surface hardness, and the surface hardness is partially Disclosed is an abrasive cloth characterized in that the different portions are formed by phase separation of the resin constituting the surface portion.
- Patent Document 2 is a polishing pad useful for flattening, and includes a polymer matrix having a glass transition temperature exceeding room temperature, in which an elastomeric polymer is dispersed, and the elastomeric polymer includes: Disclosed is a polishing pad having an average length of at least 0.1 ⁇ m in at least one direction, constituting 1 to 45% by volume of the polishing pad, and having a glass transition temperature below room temperature. ing.
- Patent Document 3 discloses a Cu film polishing polishing pad having a polishing layer made of a polyurethane resin foam for the purpose of suppressing the occurrence of scratches, the polyurethane resin foam comprising an isocyanate component and a high molecular weight polyol.
- a Cu film which is a reaction cured product of an isocyanate-terminated prepolymer containing a component as a raw material component and a chain extender, and the high molecular weight polyol component contains 30% by weight or more of a polyester polyol A polishing pad is disclosed.
- the polishing layer is an isocyanate-terminated prepolymer (A) obtained by reacting a prepolymer raw material composition (a) containing an isocyanate component and a polyester polyol, isocyanate.
- a polishing pad is disclosed in which the reaction cured body has a phase separation structure. It is described that the polishing pad has a high polishing rate, is excellent in flattening characteristics, and can suppress generation of scratches.
- An object of the present invention is to provide a polishing pad that has a polishing layer having a three-phase separation structure, has a high polishing rate, is excellent in flattening characteristics, and can suppress generation of scratches. Moreover, it aims at providing the manufacturing method of the semiconductor device using this polishing pad.
- the present invention provides a polishing pad having a polishing layer, wherein the polishing layer comprises: Isocyanate-terminated prepolymer (A) obtained by reacting a prepolymer raw material composition (a) containing an isocyanate component and a polyester-based polyol, It is formed by a reaction cured product of an isocyanate-terminated prepolymer (B) obtained by reacting a prepolymer raw material composition (b) containing an isocyanate component and a polyether polyol, and a polyurethane raw material composition containing a chain extender.
- Isocyanate-terminated prepolymer obtained by reacting a prepolymer raw material composition (a) containing an isocyanate component and a polyester-based polyol, It is formed by a reaction cured product of an isocyanate-terminated prepolymer (B) obtained by reacting a prepolymer raw material composition (b) containing an isocyanate component and a polyether poly
- the polyether polyol includes a polyether polyol (C) having a number average molecular weight of 1000 or less and a polyether polyol (D) having a number average molecular weight of 1900 or more,
- the reaction cured body relates to a polishing pad having a three-phase separation structure.
- the present inventors pay attention to the property that the polyester-based polyol and the polyether-based polyol are not compatible with each other, and use the isocyanate-terminated prepolymer (A) and the isocyanate-terminated prepolymer (B) synthesized separately as raw materials. It was found that a reaction cured product having a macroscopic three-phase separation structure can be obtained by reacting and curing these with a chain extender and the like. Then, by forming a polishing layer using the reaction cured body, the polishing rate is higher than that of the polishing pad having the two-phase separation structure described in Patent Document 4, the planarization characteristics are excellent, and the generation of scratches can be suppressed. It has been found that a polishing pad can be obtained.
- the polishing layer has a very high surface sharpening by a dressing process (cutting process) using a conditioner, thereby improving the polishing performance, so that the polishing rate is very high.
- the polishing layer as a whole has a very high hardness, and thus has excellent planarization characteristics. Since the polishing layer partially has a low hardness region due to phase separation, the generation of scratches can be effectively suppressed.
- the three-phase separation structure has a first island part, a second island part, and a sea part, the average maximum length of the first island part is 0.05 to 100 ⁇ m, and the average maximum length of the second island part The thickness is preferably 0.05 to 100 ⁇ m.
- the three-phase separation structure is a sea-island structure having a first island part, a second island part, and a sea part, the above effect is further improved.
- the first island is a soft phase
- the second island is a crystalline phase
- the sea is a hard phase.
- the 1st island part is formed with the reaction hardening body which has an isocyanate terminal prepolymer (A) as a main component, and the 2nd island part is a polycrystal among the reaction hardening body which has an isocyanate terminal prepolymer (B) as a main component. It is formed by the ether-based polyol (D) component, and the sea portion is formed by a cured portion other than the polyether-based polyol (D) component in the reaction cured body mainly composed of the isocyanate-terminated prepolymer (B). it is conceivable that.
- the second island portion which is a crystalline phase is very fragile and easily detached.
- the average maximum length of the first island is less than 0.05 ⁇ m, the effect of suppressing scratches tends to be insufficient. On the other hand, when it exceeds 100 ⁇ m, the flattening characteristics tend to deteriorate.
- the average maximum length of the second island portion is less than 0.05 ⁇ m, the surface sharpness due to the dress becomes insufficient and the polishing rate tends to be difficult to increase.
- the thickness exceeds 100 ⁇ m, the wear resistance tends to decrease, so the pad life tends to be shortened.
- the content of the polyether polyol (D) with respect to the total weight of the high molecular weight polyol contained in the prepolymer raw material compositions (a) and (b) is preferably 4 to 50% by weight.
- the content of the polyether polyol (D) is less than 4% by weight, it tends to be difficult to form a reaction cured body having a three-phase separation structure.
- it exceeds 50% by weight the proportion of the crystal phase increases, and the wear resistance tends to decrease, so the pad life tends to be shortened.
- the content of the polyether polyol (C) is preferably 100 to 1000 parts by weight with respect to 100 parts by weight of the polyether polyol (D).
- the content of the polyether-based polyol (C) is less than 100 parts by weight, the ratio of the crystal phase increases, and the wear resistance tends to decrease, so the pad life tends to be shortened, and exceeds 1000 parts by weight. In some cases, it tends to be difficult to form a reaction cured body having a three-phase separation structure.
- the polyurethane raw material composition preferably contains 50 to 500 parts by weight of the isocyanate-terminated prepolymer (B) with respect to 100 parts by weight of the isocyanate-terminated prepolymer (A).
- the isocyanate-terminated prepolymer (B) is less than 50 parts by weight, it becomes difficult to form a reaction cured body having a three-phase separation structure, and when it exceeds 500 parts by weight, the proportion of the soft phase increases and the flatness There is a tendency for the conversion characteristics to deteriorate.
- the polyester polyol is preferably at least one selected from the group consisting of polyethylene adipate glycol, polybutylene adipate glycol, and polyhexamethylene adipate glycol.
- the polyether polyols (C) and (D) are preferably polytetramethylene ether glycol.
- the present invention relates to a semiconductor device manufacturing method including a step of polishing a surface of a semiconductor wafer using the polishing pad.
- the polishing pad of the present invention has a polishing layer containing a polyurethane resin.
- the polishing pad of the present invention may be only the polishing layer or a laminate of the polishing layer and another layer (for example, a cushion layer).
- Polyurethane resin is a particularly preferable material as a material for forming the polishing layer because it has excellent wear resistance and a polymer having desired physical properties can be easily obtained by variously changing the raw material composition.
- the polishing layer is a prepolymer raw material composition comprising an isocyanate-terminated prepolymer (A) obtained by reacting a prepolymer raw material composition (a) containing an isocyanate component and a polyester polyol, an isocyanate component and a polyether polyol ( It is formed by the reaction hardening body of the polyurethane raw material composition containing the isocyanate terminal prepolymer (B) obtained by reacting b), and a chain extender, and the said reaction hardening body has a three-phase-separation structure. .
- isocyanate component a known compound in the field of polyurethane can be used without particular limitation.
- trifunctional or higher polyfunctional isocyanates may be used.
- polyester polyol examples include polyester polyols such as polyethylene adipate glycol, polypropylene adipate glycol, polybutylene adipate glycol, polyhexamethylene adipate glycol, and polycaprolactone polyol; polyester glycol such as polycaprolactone polyol and alkylene
- the reaction product with carbonate, and polyester polycarbonate polyol such as a product obtained by reacting ethylene carbonate with polyhydric alcohol and then reacting the obtained reaction mixture with organic dicarboxylic acid, and the like. These may be used alone or in combination of two or more. Among these, it is preferable to use at least one polyester polyol selected from the group consisting of polyethylene adipate glycol, polybutylene adipate glycol, and polyhexamethylene adipate glycol.
- the number average molecular weight of the polyester polyol is not particularly limited, but is preferably 200 to 5000, more preferably 500 to 2000 from the viewpoint of the three-phase separation structure and viscoelastic properties of the resulting polyurethane resin. . If the number average molecular weight is less than 200, it tends to be difficult to form a three-phase separation structure. On the other hand, when the number average molecular weight exceeds 5000, the resulting polyurethane resin becomes soft and the flattening characteristics tend to deteriorate.
- the polyester-based polyol As a high-molecular-weight polyol, but other known high-molecular-weight polyols (number-average molecular weight is within a range not impairing the object of the present invention). About 200 to 5000) may be added.
- the polyether polyol includes a polyether polyol (C) having a number average molecular weight of 1000 or less and a polyether polyol (D) having a number average molecular weight of 1900 or more.
- polyether polyol examples include polyether polyols such as polyethylene glycol (PEG), polypropylene glycol (PPG), polytetramethylene ether glycol (PTMG) and polyhexamethylene ether glycol (PHMG); 1,3- Diols such as propanediol, 1,4-butanediol, 1,6-hexanediol, polypropylene glycol and / or polytetramethylene glycol, and phosgene or diallyl carbonate (eg diphenyl carbonate) or cyclic carbonate (eg propylene carbonate) And polyether polycarbonate polyols such as the reaction product of These may be used alone or in combination of two or more. Of these, polytetramethylene ether glycol is preferably used.
- PEG polyethylene glycol
- PPG polypropylene glycol
- PTMG polytetramethylene ether glycol
- PHMG polyhexamethylene ether glycol
- the number average molecular weight of the polyether polyol (C) is preferably 850 or less.
- the number average molecular weight of the polyether-based polyol (D) is preferably 2000 or more.
- the content of the polyether polyol (C) in the prepolymer raw material composition (b) is preferably 100 to 1000 parts by weight with respect to 100 parts by weight of the polyether polyol (D).
- the content of the polyether polyol (D) is preferably 4 to 50% by weight, more preferably 5 to 5% by weight based on the total weight of the high molecular weight polyol contained in the prepolymer raw material compositions (a) and (b). 30% by weight.
- the prepolymer raw material composition (b) it is preferable to add only the polyether polyols (C) and (D) as high molecular weight polyols, but other known substances are within the range not impairing the object of the present invention.
- a high molecular weight polyol (having a number average molecular weight of about 200 to 5,000) may be added.
- low molecular weight components such as low molecular weight polyols, low molecular weight polyamines, and alcohol amines may be added.
- low molecular weight polyol examples include ethylene glycol, 1,2-propylene glycol, 1,3-propylene glycol, 1,2-butanediol, 1,3-butanediol, 1,4-butanediol, 2,3- Butanediol, 1,6-hexanediol, neopentyl glycol, 1,4-cyclohexanedimethanol, 3-methyl-1,5-pentanediol, diethylene glycol, triethylene glycol, 1,4-bis (2-hydroxyethoxy) Benzene, trimethylolpropane, glycerin, 1,2,6-hexanetriol, pentaerythritol, tetramethylolcyclohexane, methylglucoside, sorbitol, mannitol, dulcitol, sucrose, 2,2,6,6-tetrakis (hydroxymethyl) Le) cyclohexanol, diethanolamine
- low molecular weight polyamine examples include ethylenediamine, tolylenediamine, diphenylmethanediamine, and diethylenetriamine. These may be used alone or in combination of two or more.
- alcohol amine examples include monoethanolamine, 2- (2-aminoethylamino) ethanol, and monopropanolamine. These may be used alone or in combination of two or more.
- the blending amount of the low molecular weight component in the prepolymer raw material composition (b) is not particularly limited, and is appropriately determined depending on the properties required for the polishing pad (polishing layer).
- a chain extender is used for curing the prepolymer.
- the chain extender is an organic compound having two or more active hydrogen groups, and examples of the active hydrogen group include a hydroxyl group, a primary or secondary amino group, and a thiol group (SH).
- the ratio of the isocyanate-terminated prepolymer (A), the isocyanate-terminated prepolymer (B), and the chain extender can be variously changed depending on the molecular weight of each, the desired physical properties of the polishing pad, and the like.
- the addition amount of the isocyanate-terminated prepolymer (B) is preferably 50 to 500 parts by weight, more preferably 100 to 300 parts by weight, based on 100 parts by weight of the isocyanate-terminated prepolymer (A).
- the number of isocyanate groups (NCO Index) of the prepolymer relative to the number of active hydrogen groups (hydroxyl group, amino group) of the chain extender is 0.8 to 1.2. And more preferably 0.99 to 1.15. When the number of isocyanate groups is outside the above range, curing failure occurs and the required specific gravity and hardness cannot be obtained, and the polishing characteristics tend to be deteriorated.
- Polyurethane resin (reaction cured body) can be produced by applying a known urethanization technique such as a melting method or a solution method, but is preferably produced by a melting method in consideration of cost, working environment and the like.
- the polyurethane resin of the present invention is produced by a prepolymer method.
- the polyurethane resin obtained by the prepolymer method is suitable because of its excellent physical properties.
- isocyanate-terminated prepolymers (A) and (B) having a molecular weight of about 300 to 5000 are preferable because of excellent processability and physical properties.
- the polyurethane resin of the present invention is produced by reaction-curing a polyurethane raw material composition containing an isocyanate-terminated prepolymer (A), an isocyanate-terminated prepolymer (B), and a chain extender.
- the polyurethane resin may be a foam or a non-foam.
- the polyurethane resin can be produced by batch-wise measuring each component, putting it in a container, and stirring it, or continuously feeding each component to the stirring device and stirring, and then sending out the mixed solution to produce a molded product. It may be a continuous production method.
- the isocyanate-terminated prepolymers (A) and (B) are placed in a reaction vessel, and then a chain extender is added, stirred, and then poured into a casting of a predetermined size to produce a polyurethane resin block.
- the polishing layer may be manufactured by slicing using the above-mentioned method, or the polishing layer may be manufactured by processing into a thin sheet at the above-described casting stage.
- a polyurethane resin as a raw material may be dissolved and extruded from a T die to directly obtain a sheet-like polishing layer.
- Examples of methods for producing polyurethane foam include a method in which hollow beads are added, a mechanical foaming method (including a mechanical floss method), and a chemical foaming method.
- the mechanical foaming method using the silicone type surfactant which is a copolymer of polyalkylsiloxane and polyether is especially preferable.
- suitable silicone surfactants include SH-192 and L-5340 (manufactured by Toray Dow Corning Silicone), B8443, B8465 (manufactured by Goldschmidt), and the like.
- the silicone surfactant is preferably added to the polyurethane raw material composition in an amount of 0.05 to 10% by weight, more preferably 0.1 to 5% by weight.
- stabilizers such as antioxidants, lubricants, pigments, fillers, antistatic agents, and other additives may be added.
- the manufacturing method of this polyurethane foam has the following processes. 1) Foaming process for producing a cell dispersion liquid A silicone-based surfactant is added to the first component containing the isocyanate-terminated prepolymers (A) and (B) so as to be 0.05 to 10% by weight in the polyurethane foam. Then, stirring is performed in the presence of a non-reactive gas, and the non-reactive gas is dispersed as fine bubbles to obtain a bubble dispersion. When the prepolymer is solid at normal temperature, it is preheated to an appropriate temperature and melted before use.
- non-reactive gas used to form the fine bubbles non-flammable gases are preferable, and specific examples include nitrogen, oxygen, carbon dioxide, rare gases such as helium and argon, and mixed gases thereof. In view of cost, it is most preferable to use air that has been dried to remove moisture.
- a known stirring device can be used without particular limitation as a stirring device for dispersing non-reactive gas in the form of fine bubbles and dispersed in the first component containing the silicone-based surfactant.
- a shaft planetary mixer (planetary mixer) is exemplified.
- the shape of the stirring blade of the stirring device is not particularly limited, but it is preferable to use a whipper type stirring blade because fine bubbles can be obtained.
- the rotational speed of the stirring blade is preferably 500 to 2000 rpm, more preferably 800 to 1500 rpm.
- the stirring time is appropriately adjusted according to the target density.
- the stirring in the mixing step may not be stirring that forms bubbles, and it is preferable to use a stirring device that does not involve large bubbles.
- a planetary mixer is suitable. There is no problem even if the same stirring device is used as the stirring device for the foaming step and the mixing step, and it is also preferable to adjust the stirring conditions such as adjusting the rotation speed of the stirring blade as necessary. .
- the foam reaction solution may be poured into the mold and immediately put into a heating oven for post cure, and heat is not immediately transferred to the reaction components under such conditions, so the bubble size does not increase.
- the curing reaction is preferably performed at normal pressure because the bubble shape is stable.
- stimulates well-known polyurethane reactions such as a tertiary amine type
- the type and addition amount of the catalyst are selected in consideration of the flow time for pouring into a mold having a predetermined shape after the mixing step.
- the average cell diameter of the polyurethane foam is preferably 20 to 70 ⁇ m, more preferably 30 to 60 ⁇ m.
- the Asker D hardness is preferably 35 to 65 degrees, more preferably 40 to 65 degrees.
- the Asker D hardness is preferably 45 to 75 degrees, more preferably 45 to 65 degrees.
- the specific gravity of the polyurethane foam is preferably 0.4 to 1.0.
- the polishing layer made of the polyurethane resin has a three-phase separation structure.
- the three-phase separation structure has a first island part, a second island part, and a sea part.
- the average maximum length of the first island part is 0.05 to 100 ⁇ m
- the average maximum of the second island part is The length is preferably 0.05 to 100 ⁇ m.
- the polishing surface of the polishing pad (polishing layer) of the present invention that comes into contact with the material to be polished preferably has a concavo-convex structure for holding and updating the slurry.
- the polishing layer made of foam has many openings on the polishing surface and has the function of holding and updating the slurry.
- the slurry can be held and updated more efficiently. It can be performed well, and destruction of the material to be polished due to adsorption with the material to be polished can be prevented.
- the concavo-convex structure is not particularly limited as long as it is a shape that holds and renews the slurry.
- an XY lattice groove for example, an XY lattice groove, a concentric circular groove, a through hole, a non-penetrating hole, a polygonal column, a cylinder, a spiral groove, Examples include eccentric circular grooves, radial grooves, and combinations of these grooves.
- these uneven structures are generally regular, but in order to make the slurry retention and renewability desirable, the groove pitch, groove width, groove depth, etc. should be changed for each range. Is also possible.
- the method for producing the concavo-convex structure is not particularly limited.
- a method of machine cutting using a jig such as a tool of a predetermined size, pouring a resin into a mold having a predetermined surface shape, and curing.
- a method of producing a resin by pressing a method of producing using photolithography, a method of producing using a printing technique, a carbon dioxide laser, etc.
- Examples include a manufacturing method using laser light.
- the thickness of the polishing layer is not particularly limited, but is usually about 0.8 to 4 mm, preferably 1.5 to 2.5 mm.
- a method for producing the polishing layer having the above thickness a method in which the block of the fine foam is made to have a predetermined thickness using a band saw type or canna type slicer, a resin is poured into a mold having a cavity having a predetermined thickness, and curing is performed. And a method using a coating technique or a sheet forming technique.
- the polishing pad of the present invention may be a laminate of the polishing layer and a cushion sheet.
- the cushion sheet (cushion layer) supplements the characteristics of the polishing layer.
- the cushion sheet is necessary for achieving both planarity and uniformity in a trade-off relationship in CMP.
- Planarity refers to the flatness of a pattern portion when a material having fine irregularities generated during pattern formation is polished, and uniformity refers to the uniformity of the entire material to be polished.
- the planarity is improved by the characteristics of the polishing layer, and the uniformity is improved by the characteristics of the cushion sheet.
- cushion sheet examples include fiber nonwoven fabrics such as polyester nonwoven fabric, nylon nonwoven fabric and acrylic nonwoven fabric, resin-impregnated nonwoven fabrics such as polyester nonwoven fabric impregnated with polyurethane, polymer resin foams such as polyurethane foam and polyethylene foam, butadiene rubber, and isoprene.
- fiber nonwoven fabrics such as polyester nonwoven fabric, nylon nonwoven fabric and acrylic nonwoven fabric
- resin-impregnated nonwoven fabrics such as polyester nonwoven fabric impregnated with polyurethane
- polymer resin foams such as polyurethane foam and polyethylene foam
- butadiene rubber butadiene rubber
- isoprene examples include rubber resins such as rubber and photosensitive resins.
- Examples of means for attaching the polishing layer and the cushion sheet include a method of sandwiching and pressing the polishing layer and the cushion sheet with a double-sided tape.
- the double-sided tape has a general configuration in which adhesive layers are provided on both sides of a substrate such as a nonwoven fabric or a film. In consideration of preventing the penetration of the slurry into the cushion sheet, it is preferable to use a film for the substrate.
- the polishing pad of the present invention may be provided with a double-sided tape on the surface to be bonded to the platen.
- a double-sided tape a tape having a general configuration in which an adhesive layer is provided on both surfaces of a base material can be used as described above.
- a base material a nonwoven fabric, a film, etc. are mentioned, for example.
- the semiconductor device is manufactured through a process of polishing the surface of the semiconductor wafer using the polishing pad.
- a semiconductor wafer is generally a laminate of a wiring metal and an oxide film on a silicon wafer.
- the method and apparatus for polishing the semiconductor wafer are not particularly limited.
- a polishing surface plate 2 that supports a polishing pad (polishing layer) 1 and a support table (polishing head) that supports the semiconductor wafer 4. 5 and a polishing apparatus equipped with a backing material for uniformly pressing the wafer and a supply mechanism of the abrasive 3.
- the polishing pad 1 is attached to the polishing surface plate 2 by attaching it with a double-sided tape, for example.
- the polishing surface plate 2 and the support base 5 are disposed so that the polishing pad 1 and the semiconductor wafer 4 supported on each of the polishing surface plate 2 and the support table 5 face each other, and are provided with rotating shafts 6 and 7 respectively. Further, a pressurizing mechanism for pressing the semiconductor wafer 4 against the polishing pad 1 is provided on the support base 5 side. In polishing, the semiconductor wafer 4 is pressed against the polishing pad 1 while rotating the polishing surface plate 2 and the support base 5, and polishing is performed while supplying slurry.
- the flow rate of the slurry, the polishing load, the polishing platen rotation speed, and the wafer rotation speed are not particularly limited and are appropriately adjusted.
- the protruding portion of the surface of the semiconductor wafer 4 is removed and polished flat. Thereafter, a semiconductor device is manufactured by dicing, bonding, packaging, or the like. The semiconductor device is used for an arithmetic processing device, a memory, and the like.
- the produced polyurethane foam was cut out (arbitrary size), and a smooth surface was cut out with a diamond knife using an ultramicrotome (Leica EM UC6, manufactured by Leica) in an environment of ⁇ 80 ° C.
- the produced polyurethane foam was cut as thin as possible to a thickness of 1 mm or less in parallel with a microtome cutter, and used as a sample for measuring the average cell diameter.
- the sample was fixed on a glass slide and observed at 100 times using SEM (S-3500N, Hitachi Science Systems, Ltd.).
- SEM S-3500N, Hitachi Science Systems, Ltd.
- the image analysis software WinRoof, Mitani Shoji Co., Ltd.
- polishing characteristics were evaluated using the prepared polishing pad.
- the polishing rate was calculated from the polishing amount obtained by polishing a thermal oxide film of 1 ⁇ m formed on an 8-inch silicon wafer for 60 seconds.
- An optical interference type film thickness measuring device manufactured by Nanometrics, device name: Nanospec was used for measuring the thickness of the oxide film.
- silica slurry SS12 Cabot was added as a slurry at a flow rate of 150 ml / min during polishing.
- the polishing load was 350 g / cm 2
- the polishing platen rotation number was 35 rpm
- the wafer rotation number was 30 rpm.
- the flattening characteristics were evaluated by the amount of scraping. After depositing a thermal oxide film of 0.5 ⁇ m on an 8-inch silicon wafer and performing predetermined patterning, an oxide film of 1 ⁇ m was deposited by p-TEOS to produce a patterned wafer having an initial step of 0.5 ⁇ m. This wafer was polished under the above conditions, and after polishing, each step was measured to calculate the amount of scraping.
- the amount of scraping is 270 ⁇ m when the step of the upper part of the lines of the two types of patterns is 2000 mm or less in a pattern in which 270 ⁇ m wide lines are arranged in a 30 ⁇ m space and a pattern in which 30 ⁇ m wide lines are arranged in a 270 ⁇ m space This is the amount of space shaving.
- the amount of scraping of the space of 270 ⁇ m is small, the amount of shaving of the portion that is not desired to be shaved is small, indicating that the flatness is high.
- 88 parts by weight of isophorone diisocyanate 53 parts by weight of polytetramethylene ether glycol having a number average molecular weight of 2000
- number average molecular weight A mixture of 106 parts by weight of 1000 polytetramethylene ether glycol, 103 parts by weight of polytetramethylene ether glycol having a number average molecular weight of 650, and 258 parts by weight of polytetramethylene ether glycol having a number average molecular weight of 250 was allowed to react at 70 ° C. for 4 hours.
- An isocyanate-terminated prepolymer (B) was obtained. 33 parts by weight of the prepolymer (A), 67 parts by weight of the prepolymer (B), and 3 parts by weight of a silicone surfactant (manufactured by Goldschmidt, B8465) are added to the polymerization vessel and mixed to 70 ° C. Adjusted and degassed under reduced pressure. Then, it stirred vigorously for about 4 minutes so that a bubble might be taken in in a reaction system with the rotation speed of 900 rpm using the stirring blade. To this, 27.2 parts by weight of 4,4′-methylenebis (o-chloroaniline) previously melted at 120 ° C. was added (NCO Index: 1.1).
- the mixed liquid was stirred for about 70 seconds, and then poured into a pan-shaped open mold (casting container). When the fluidity of the mixed solution disappeared, it was put in an oven and post-cured at 100 ° C. for 16 hours to obtain a polyurethane foam block.
- the polyurethane foam block heated to about 80 ° C. was sliced using a slicer (AGW) and VGW-125 to obtain a polyurethane foam sheet. Next, using a buffing machine (Amitech Co., Ltd.), the surface of the sheet was buffed to a thickness of 1.27 mm to obtain a sheet with an adjusted thickness accuracy.
- the buffed sheet is punched out with a diameter of 61 cm, and a concentric circle having a groove width of 0.25 mm, a groove pitch of 1.50 mm, and a groove depth of 0.40 mm on the surface using a groove processing machine (manufactured by Techno). Groove processing was performed to obtain a polishing layer.
- the surface of the polishing layer had a sea-island structure having a first island part, a second island part, and a sea part, and the shape of the first island part and the second island part was circular (see FIG. 2).
- a double-sided tape (manufactured by Sekisui Chemical Co., Ltd., double tack tape) was attached to the surface of the polishing layer opposite to the grooved surface using a laminator. Furthermore, the surface of the corona-treated cushion sheet (manufactured by Toray Industries, Inc., polyethylene foam, Torepef, thickness 0.8 mm) was buffed and bonded to the double-sided tape using a laminator. Further, a double-sided tape was attached to the other surface of the cushion sheet using a laminator to prepare a polishing pad.
- Example 2 and 3 Comparative Example 1 A polishing pad was prepared in the same manner as in Example 1 except that the formulation shown in Table 1 was adopted.
- the polishing layers of Examples 2 and 3 had a three-phase separation structure having a first island part, a second island part, and a sea part.
- FIG. 3 is an image (30 ⁇ m ⁇ 30 ⁇ m and 5 ⁇ m ⁇ 5 ⁇ m) obtained by measuring the surface of the polishing layer produced in Example 2 with a scanning probe microscope.
- the polishing layer of Comparative Example 1 had a two-phase separation structure having an island part and a sea part.
- the polishing pad of the present invention provides stable and high polishing for flattening of optical materials such as lenses and reflection mirrors, silicon wafers, aluminum substrates, and materials requiring high surface flatness such as general metal polishing. Can be done with efficiency.
- the polishing pad of the present invention is particularly suitable for a step of planarizing a silicon wafer and a device having an oxide layer, a metal layer, etc. formed thereon, before further laminating and forming these oxide layers and metal layers. Can be used for
- polishing pad polishing layer
- polishing surface plate Abrasive (slurry)
- Material to be polished semiconductor wafer
- Support base (polishing head) 6
- Rotating shaft Rotating shaft
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Abstract
Description
イソシアネート成分及びポリエステル系ポリオールを含むプレポリマー原料組成物(a)を反応して得られるイソシアネート末端プレポリマー(A)、
イソシアネート成分及びポリエーテル系ポリオールを含むプレポリマー原料組成物(b)を反応して得られるイソシアネート末端プレポリマー(B)、及び
鎖延長剤を含むポリウレタン原料組成物の反応硬化体により形成されており、
前記ポリエーテル系ポリオールは、数平均分子量1000以下のポリエーテル系ポリオール(C)及び数平均分子量1900以上のポリエーテル系ポリオール(D)を含み、
前記反応硬化体は3相分離構造を有することを特徴とする研磨パッド、に関する。
1)気泡分散液を作製する発泡工程
イソシアネート末端プレポリマー(A)及び(B)を含む第1成分にシリコーン系界面活性剤をポリウレタン発泡体中に0.05~10重量%になるように添加し、非反応性気体の存在下で撹拌し、非反応性気体を微細気泡として分散させて気泡分散液とする。前記プレポリマーが常温で固体の場合には適宜の温度に予熱し、溶融して使用する。
2)硬化剤(鎖延長剤)混合工程
上記の気泡分散液に鎖延長剤を含む第2成分を添加、混合、撹拌して発泡反応液とする。
3)注型工程
上記の発泡反応液を金型に流し込む。
4)硬化工程
金型に流し込まれた発泡反応液を加熱し、反応硬化させる。
(数平均分子量の測定)
数平均分子量は、GPC(ゲル・パーミエーション・クロマトグラフィ)にて測定し、標準ポリスチレンにより換算した。
GPC装置:島津製作所製、LC-10A
カラム:Polymer Laboratories社製、(PLgel、5μm、500Å)、(PLgel、5μm、100Å)、及び(PLgel、5μm、50Å)の3つのカラムを連結して使用
流量:1.0ml/min
濃度:1.0g/l
注入量:40μl
カラム温度:40℃
溶離液:テトラヒドロフラン
作製したポリウレタン発泡体を切り出し(大きさ任意)、-80℃の環境下において、ウルトラミクロトーム(ライカ社製、LEICA EM UC6)を用いて、ダイヤモンドナイフにて平滑面を切り出した。その後、走査型プローブ顕微鏡(島津製作所製、SPM-9500)及びカンチレバー(オリンパス社製、OMCL-AC200TS-R3、ばね定数:9N/m、共振周波数:150Hz)を用い、カンチレバーの走査速度1Hz、測定温度23℃の条件下で、粘弾性測定システムの位相検出モードにて当該平滑面(測定範囲:30μm×30μm及び5μm×5μm)を測定した。得られた画像の濃淡範囲を2Vとした際に、濃淡により島部が明確に判断できる画像を画像解析ソフト(WinRoof、三谷商事(株))を用いて表示し、測定範囲30μm×30μm及び5μm×5μmにおける第1島部10個及び第2島部10個の最大長さをそれぞれ測定し、それらの値から平均最大長さを算出した。
作製したポリウレタン発泡体を厚み1mm以下になるべく薄くミクロトームカッターで平行に切り出したものを平均気泡径測定用試料とした。試料をスライドガラス上に固定し、SEM(S-3500N、日立サイエンスシステムズ(株))を用いて100倍で観察した。得られた画像を画像解析ソフト(WinRoof、三谷商事(株))を用いて、任意範囲の全気泡径を測定し、平均気泡径(μm)を算出した。
JIS K6253-1997に準拠して行った。作製したポリウレタン発泡体を2cm×2cm(厚み:任意)の大きさに切り出したものを硬度測定用試料とし、温度23℃±2℃、湿度50%±5%の環境で16時間静置した。測定時には、試料を重ね合わせ、厚み6mm以上とした。硬度計(高分子計器社製、アスカーD型硬度計)を用い、任意の10箇所における硬度を測定し、その平均値を求めた。
JIS Z8807-1976に準拠して行った。作製したポリウレタン発泡体を4cm×8.5cmの短冊状(厚み:任意)に切り出したものを比重測定用試料とし、温度23℃±2℃、湿度50%±5%の環境で16時間静置した。測定には比重計(ザルトリウス社製)を用い、比重を測定した。
研磨装置としてSPP600S(岡本工作機械社製)を用い、作製した研磨パッドを用いて、研磨特性の評価を行った。研磨速度は、8インチのシリコンウエハに熱酸化膜を1μm製膜したものを、60秒研磨してこのときの研磨量より算出した。酸化膜の膜厚測定には、光干渉式膜厚測定装置(ナノメトリクス社製、装置名:Nanospec)を用いた。研磨条件としては、スラリーとして、シリカスラリー(SS12 キャボット社製)を研磨中に流量150ml/min添加した。研磨荷重としては350g/cm2、研磨定盤回転数35rpm、ウエハ回転数30rpmとした。
容器にトルエンジイソシアネート(2,4-体/2,6-体=80/20の混合物)259重量部、及び数平均分子量1000のポリエチレンアジペートグリコール741重量部を入れ、70℃で4時間反応させてイソシアネート末端プレポリマー(A)を得た。
容器にトルエンジイソシアネート(2,4-体/2,6-体=80/20の混合物)392重量部、イソホロンジイソシアネート88重量部、数平均分子量2000のポリテトラメチレンエーテルグリコール53重量部、数平均分子量1000のポリテトラメチレンエーテルグリコール106重量部、数平均分子量650のポリテトラメチレンエーテルグリコール103重量部、及び数平均分子量250のポリテトラメチレンエーテルグリコール258重量部を入れ、70℃で4時間反応させてイソシアネート末端プレポリマー(B)を得た。
前記プレポリマー(A)33重量部、前記プレポリマー(B)67重量部、及びシリコーン系界面活性剤(ゴールドシュミット社製、B8465)3重量部を重合容器内に加えて混合し、70℃に調整して減圧脱泡した。その後、撹拌翼を用いて、回転数900rpmで反応系内に気泡を取り込むように激しく約4分間撹拌を行った。そこへ予め120℃に溶融した4,4’-メチレンビス(o-クロロアニリン)27.2重量部を添加した(NCO Index:1.1)。該混合液を約70秒間撹拌した後、パン型のオープンモールド(注型容器)へ流し込んだ。この混合液の流動性がなくなった時点でオーブン内に入れ、100℃で16時間ポストキュアを行い、ポリウレタン発泡体ブロックを得た。
約80℃に加熱した前記ポリウレタン発泡体ブロックをスライサー(アミテック社製、VGW-125)を使用してスライスし、ポリウレタン発泡体シートを得た。次に、バフ機(アミテック社製)を使用して、厚さ1.27mmになるまで該シートの表面バフ処理をし、厚み精度を整えたシートとした。このバフ処理をしたシートを直径61cmの大きさで打ち抜き、溝加工機(テクノ社製)を用いて表面に溝幅0.25mm、溝ピッチ1.50mm、溝深さ0.40mmの同心円状の溝加工を行い研磨層を得た。研磨層表面は、第1島部と第2島部と海部とを有する海島構造であり、第1島部と第2島部の形状は円形であった(図2参照)。この研磨層の溝加工面と反対側の面にラミ機を使用して、両面テープ(積水化学工業社製、ダブルタックテープ)を貼りつけた。更に、コロナ処理をしたクッションシート(東レ社製、ポリエチレンフォーム、トーレペフ、厚み0.8mm)の表面をバフ処理し、それを前記両面テープにラミ機を使用して貼り合わせた。さらに、クッションシートの他面にラミ機を使用して両面テープを貼り合わせて研磨パッドを作製した。
表1に記載の配合を採用した以外は実施例1と同様の方法で研磨パッドを作製した。実施例2及び3の研磨層は第1島部と第2島部と海部とを有する3相分離構造であった。図3は、実施例2で作製した研磨層の表面を走査型プローブ顕微鏡で測定した画像(30μm×30μm及び5μm×5μm)である。比較例1の研磨層は島部と海部とを有する2相分離構造であった。
2:研磨定盤
3:研磨剤(スラリー)
4:被研磨材(半導体ウエハ)
5:支持台(ポリシングヘッド)
6、7:回転軸
Claims (8)
- 研磨層を有する研磨パッドにおいて、前記研磨層は、
イソシアネート成分及びポリエステル系ポリオールを含むプレポリマー原料組成物(a)を反応して得られるイソシアネート末端プレポリマー(A)、
イソシアネート成分及びポリエーテル系ポリオールを含むプレポリマー原料組成物(b)を反応して得られるイソシアネート末端プレポリマー(B)、及び
鎖延長剤を含むポリウレタン原料組成物の反応硬化体により形成されており、
前記ポリエーテル系ポリオールは、数平均分子量1000以下のポリエーテル系ポリオール(C)及び数平均分子量1900以上のポリエーテル系ポリオール(D)を含み、
前記反応硬化体は3相分離構造を有することを特徴とする研磨パッド。 - 3相分離構造は、第1島部と第2島部と海部を有しており、第1島部の平均最大長さが0.05~100μmであり、第2島部の平均最大長さが0.05~100μmである請求項1記載の研磨パッド。
- プレポリマー原料組成物(a)及び(b)に含まれる高分子量ポリオール全重量に対するポリエーテル系ポリオール(D)の含有量が4~50重量%である請求項1又は2記載の研磨パッド。
- ポリエーテル系ポリオール(C)の含有量は、ポリエーテル系ポリオール(D)100重量部に対して100~1000重量部である請求項1~3のいずれかに記載の研磨パッド。
- ポリウレタン原料組成物は、イソシアネート末端プレポリマー(A)100重量部に対してイソシアネート末端プレポリマー(B)を50~500重量部含有する請求項1~4のいずれかに記載の研磨パッド。
- ポリエステル系ポリオールは、ポリエチレンアジペートグリコール、ポリブチレンアジペートグリコール、及びポリヘキサメチレンアジペートグリコールからなる群より選択される少なくとも1種である請求項1~5のいずれかに記載の研磨パッド。
- ポリエーテル系ポリオール(C)及び(D)は、ポリテトラメチレンエーテルグリコールである請求項1~6のいずれかに記載の研磨パッド。
- 請求項1~7のいずれかに記載の研磨パッドを用いて半導体ウエハの表面を研磨する工程を含む半導体デバイスの製造方法。
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CN201480004696.3A CN104918750A (zh) | 2013-01-31 | 2014-01-17 | 抛光垫 |
KR1020157014801A KR20150081351A (ko) | 2013-01-31 | 2014-01-17 | 연마 패드 |
SG11201505923QA SG11201505923QA (en) | 2013-01-31 | 2014-01-17 | Polishing pad |
US14/761,297 US20150360342A1 (en) | 2013-01-31 | 2014-01-17 | Polishing pad |
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WO2022153961A1 (ja) * | 2021-01-14 | 2022-07-21 | 富士紡ホールディングス株式会社 | 研磨パッド、研磨パッドの製造方法、及び光学材料又は半導体材料の表面を研磨する方法 |
CN116000799B (zh) * | 2022-12-20 | 2023-09-22 | 南通北风橡塑制品有限公司 | 一种防静电聚氨酯抛光垫及其制备方法 |
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JP2000263423A (ja) * | 1999-03-16 | 2000-09-26 | Toray Ind Inc | 研磨パッドおよび研磨装置 |
JP2007204651A (ja) * | 2006-02-03 | 2007-08-16 | Kuraray Co Ltd | 研磨パッドおよびその製造方法 |
JP2010082719A (ja) * | 2008-09-30 | 2010-04-15 | Fujibo Holdings Inc | 研磨パッドおよびその製造方法 |
JP2012000745A (ja) * | 2010-05-19 | 2012-01-05 | Toyo Tire & Rubber Co Ltd | 研磨パッド |
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WO2002046283A1 (fr) * | 2000-12-08 | 2002-06-13 | Kuraray. Co., Ltd. | Mousse de polyurethane thermoplastique, son procede de fabrication et tampons de polissage a base de cette mousse |
KR100790427B1 (ko) * | 2001-04-09 | 2008-01-02 | 도요 고무 고교 가부시키가이샤 | 폴리우레탄 조성물 및 연마 패드 |
TWI313693B (en) * | 2002-12-17 | 2009-08-21 | Dainippon Ink & Chemicals | Two-component curable polyol composition for foamed grindstone, two-component curable composition for foamed grindstone, foamed grindstone, and method for producing foamed grindstone |
US20050171224A1 (en) * | 2004-02-03 | 2005-08-04 | Kulp Mary J. | Polyurethane polishing pad |
JP4475404B2 (ja) * | 2004-10-14 | 2010-06-09 | Jsr株式会社 | 研磨パッド |
JP5634903B2 (ja) * | 2010-02-25 | 2014-12-03 | 東洋ゴム工業株式会社 | 研磨パッド |
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JP2000263423A (ja) * | 1999-03-16 | 2000-09-26 | Toray Ind Inc | 研磨パッドおよび研磨装置 |
JP2007204651A (ja) * | 2006-02-03 | 2007-08-16 | Kuraray Co Ltd | 研磨パッドおよびその製造方法 |
JP2010082719A (ja) * | 2008-09-30 | 2010-04-15 | Fujibo Holdings Inc | 研磨パッドおよびその製造方法 |
JP2012000745A (ja) * | 2010-05-19 | 2012-01-05 | Toyo Tire & Rubber Co Ltd | 研磨パッド |
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CN104918750A (zh) | 2015-09-16 |
TWI515240B (zh) | 2016-01-01 |
US20150360342A1 (en) | 2015-12-17 |
SG11201505923QA (en) | 2015-08-28 |
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