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WO2025206235A1 - Corps en résine poreux, tampon de polissage de semi-conducteur composé et procédé de fabrication de corps en résine poreux - Google Patents

Corps en résine poreux, tampon de polissage de semi-conducteur composé et procédé de fabrication de corps en résine poreux

Info

Publication number
WO2025206235A1
WO2025206235A1 PCT/JP2025/012613 JP2025012613W WO2025206235A1 WO 2025206235 A1 WO2025206235 A1 WO 2025206235A1 JP 2025012613 W JP2025012613 W JP 2025012613W WO 2025206235 A1 WO2025206235 A1 WO 2025206235A1
Authority
WO
WIPO (PCT)
Prior art keywords
resin
thin plate
polishing
organic solvent
molded body
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/JP2025/012613
Other languages
English (en)
Japanese (ja)
Inventor
誠 佐藤
速水 麻子 成瀬
久徳 黒部
敬 上野
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Noritake Co Ltd
Original Assignee
Noritake Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from JP2024052459A external-priority patent/JP7637467B1/ja
Priority claimed from JP2024052458A external-priority patent/JP7571326B1/ja
Application filed by Noritake Co Ltd filed Critical Noritake Co Ltd
Publication of WO2025206235A1 publication Critical patent/WO2025206235A1/fr
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

Links

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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/20—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
    • B24D3/22—Rubbers synthetic or natural
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/26—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a solid phase from a macromolecular composition or article, e.g. leaching out
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting

Definitions

  • the gist of the sixth invention is (1) a method for producing a resin porous body having high oxidant resistance and abrasion resistance and fine pores, comprising: (2) a melt preparation step of melting a base resin and a disaccharide, which are highly resistant to oxidants and abrasion, in an organic solvent to obtain a melt; (3) a molding step of molding the melt into a thin plate to obtain a thin plate-like molded body; (4) a precipitation step of leaving the thin plate-like molded body in cold water whose temperature is lower than the melting point of the disaccharide to precipitate fine solids of the disaccharide in the thin plate-like molded body; (5) a substitution step of leaving the thin plate-like molded body that has undergone the precipitation step in warm water whose temperature is higher than the cold water to substitute the finely precipitated disaccharide solids in the thin plate-like molded body and the organic solvent in the thin plate-like molded body with water; and (6) a drying step of drying the thin plate-
  • the gist of the seventh invention is that in the fifth or sixth invention, the base resin is PES (polyethersulfone) resin or PVDF-HFP (a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene) resin.
  • PES polyethersulfone
  • PVDF-HFP a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene
  • the gist of the tenth invention is that, in the fifth invention, the high-melting-point organic solvent is a solvent that disperses in water and dissolves the PES (polyethersulfone) resin and the PVDF-HFP (a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene) resin.
  • the high-melting-point organic solvent is a solvent that disperses in water and dissolves the PES (polyethersulfone) resin and the PVDF-HFP (a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene) resin.
  • the gist of the eleventh invention is that, in the sixth invention, the organic solvent is a solvent that disperses in water and dissolves the PES (polyethersulfone) resin and the PVDF-HFP (a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene) resin.
  • the organic solvent is a solvent that disperses in water and dissolves the PES (polyethersulfone) resin and the PVDF-HFP (a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene) resin.
  • the gist of the thirteenth invention is that, in the fifth invention, the resin porous body has micropores with an average diameter of 2 to 20 ⁇ m, preferably 2 to 10 ⁇ m.
  • the porous resin body of the first invention is a PES (polyethersulfone) resin or PVDF-HFP (a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene) resin, which has high resistance to oxidizing agents and abrasion, and has micropores formed within the base resin with a size of 0.2 to 20 ⁇ m.
  • PES polyethersulfone
  • PVDF-HFP a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene
  • the porous resin body of the third invention is a porous resin body in which the size of the micropores formed within the base resin is 0.2 to 3 ⁇ m. Therefore, when used as the base resin of a compound semiconductor polishing pad for CMP polishing of a difficult-to-polish wafer, which uses a polishing solution that mechanically promotes polishing while also promoting chemical polishing, a compound semiconductor polishing pad can be obtained that is free of scratches and can maintain its polishing rate and surface roughness for a long period of time.
  • the compound semiconductor polishing pad of the fourth invention has a base resin composed of the porous resin body of the first invention. Therefore, when used to polish hard-to-polish compound semiconductor wafers by the CMP method using a polishing solution containing a permanganate-based strong oxidizing agent, there are no scratches and the polishing rate and surface roughness can be maintained for a long period of time.
  • the gist of the fifth invention is (1) a method for producing a resin porous body having high oxidant resistance and abrasion resistance and micropores, comprising: (2) a melt preparation step of melting a base resin having high oxidant resistance and abrasion resistance in an organic solvent to obtain a melt; (3) a molding step of molding the melt into a thin plate to obtain a thin plate-like molded body; (4) a precipitation step of leaving the thin plate-like molded body in cold water to cause fine precipitation of a solid of the high-melting point organic solvent in the thin plate-like molded body; (5) a substitution step of leaving the thin plate-like molded body that has undergone the precipitation step in warm water that is higher in temperature than the cold water to replace the organic solvent that has finely precipitated in the thin plate-like molded body with water; and (6) a drying step of drying the thin plate-like molded body until all moisture is removed from the thin plate-like molded body.
  • the gist of the sixth invention is that, in the fifth invention, (2') in the melt preparation step, the base resin is melted in a high-melting-point organic solvent that has a melting point at room temperature (10-30°C) and is soluble in water to obtain a melt; (4') in the precipitation step, the thin plate-shaped molded body is left in cold water that is lower than the melting point of the high-melting-point organic solvent to precipitate fine solids of the high-melting-point organic solvent in the thin plate-shaped molded body; and (5') in the substitution step, the thin plate-shaped molded body that has undergone the precipitation step is left in warm water that is higher than the temperature of the cold water and the melting point of the high-melting-point organic solvent to replace the finely precipitated solids of the high-melting-point organic solvent in the thin plate-shaped molded body with water.
  • the gist of the seventh invention is that, in the fifth invention, (2'') in the melt preparation step, a base resin and a disaccharide having high resistance to oxidizing agents and wear are melted in an organic solvent to obtain a melt; (4'') in the precipitation step, the thin plate-shaped body is left in cold water at a temperature lower than the melting point of the disaccharide to precipitate fine solids of the disaccharide in the thin plate-shaped body; and (5) in the replacement step, the finely precipitated solids of the disaccharide in the thin plate-shaped body and the organic solvent in the thin plate-shaped body are replaced with water.
  • the base resin is PES (polyethersulfone) resin or PVDF-HFP (a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene) resin, resulting in a porous resin body with high resistance to oxidizing agents and abrasion.
  • PES polyethersulfone
  • PVDF-HFP a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene
  • the organic solvent is N-methyl-2-pyrrolidone or 2-pyrrolidone. If room temperature is defined as 10°C to 30°C, N-methyl-2-pyrrolidone has a melting point below freezing, while 2-pyrrolidone has a melting point at room temperature.
  • These organic solvents dissolve the base resins, PES (polyethersulfone) resin and PVDF-HFP (a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene), as well as lactose.
  • the high-melting-point organic solvent is a solvent that disperses in water and dissolves PES (polyethersulfone) resin and PVDF-HFP resin. This allows the thin plate-shaped molded body that has undergone the precipitation process to be left in warm water that is higher than the temperature of the cold water and the melting point of the high-melting-point organic solvent, and the finely precipitated solid high-melting-point organic solvent in the thin plate-shaped molded body can be replaced with water.
  • PES polyethersulfone
  • the organic solvent is a solvent that disperses in water and dissolves PES (polyethersulfone) resin and PVDF-HFP (a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene) resin.
  • PES polyethersulfone
  • PVDF-HFP a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene
  • the precipitation step involves leaving the thin plate-shaped body in cold water at 5 to 10°C
  • the replacement step involves leaving the thin plate-shaped body that has undergone the precipitation step in warm water at 40 to 60°C, which is sufficiently higher than the melting point of the high-melting-point organic solvent. This allows the high-melting-point organic solvent solid to be finely precipitated in the thin plate-shaped body, and then the high-melting-point organic solvent solid that has precipitated in the thin plate-shaped body is replaced with water in the warm water.
  • the porous resin body has micropores with an average diameter of 0.2 to 3 ⁇ m. This has the advantage that when polishing a hard-to-polish compound semiconductor wafer with a compound semiconductor polishing pad made of a porous resin body, the edges of the numerous micropores contribute to the polishing mechanism, making it difficult for scratches to occur, and achieving an optimal polishing rate and surface roughness.
  • the compound semiconductor polishing pad of the fourth invention has 54.3 to 65.1 volume % pores, 34.9 to 45.7 volume % PES resin, and a durometer hardness of 34.0 to 54.0, so it is free from scratches and can maintain its polishing rate and surface roughness for a long period of time.
  • FIG. 2 is a diagram showing the chemical structure of PVDF-HFP resin (80% polyvinylidene fluoride + 20% propylene hexafluoride copolymer resin), which is another example of the resin constituting the polishing pad of FIG. 1.
  • FIG. 1 is a table showing samples used in polishing test 1 and the results of the polishing test. 1 is a table showing the resin proportion, pore proportion, and durometer hardness of Examples 1 to 4 in the samples used in Polishing Test 1.
  • This is a SEM photograph of a cross section of Example Product 3 in the sample used in Polishing Test 1, showing pores in Example Product 3.
  • the workpiece 16 is held on the lower surface of the application disc 20, i.e., the surface facing the polishing pad 18, and the application disc 20 presses the workpiece 16 against the polishing pad 18 with a predetermined load.
  • a drip nozzle 22 is provided near the application disc 20 of the surface polishing device 10, and a strongly acidic polishing liquid PF containing an added strong oxidizing agent of permanganate such as potassium permanganate ( KMnO4 ) is supplied from a tank (not shown) onto the polishing surface plate 12.
  • the surface polishing apparatus 10 is optionally equipped with an adjustment tool holding member (not shown) that is rotatable about the rotation axis C1 of the polishing table 12 and movable in the direction of the rotation axis C1 and radially around the polishing table 12, and an abrasive body adjustment tool (dresser or conditioner) such as a diamond wheel (not shown) that is attached to the underside of the adjustment tool holding member, i.e., the surface facing the polishing pad 18.
  • an adjustment tool holding member (not shown) that is rotatable about the rotation axis C1 of the polishing table 12 and movable in the direction of the rotation axis C1 and radially around the polishing table 12
  • an abrasive body adjustment tool dressing or conditioner
  • a diamond wheel not shown
  • This adjustment tool holding member and the abrasive body adjustment tool attached to it are pressed against the polishing pad 18 while being rotated and driven by an adjustment tool drive motor (not shown), and are moved back and forth radially around the polishing table 12, thereby adjusting the polishing surface of the polishing pad 18 and constantly maintaining the surface condition of the polishing pad 18 in a state suitable for polishing.
  • the application disk 20 is rotated about the rotation axis C2 by the rotational force based on the difference in peripheral speed between the polishing table 12 and the polishing pad 18, and the application disk 20 is pressed against the polishing pad 18 on the polishing table 12 by the load of, for example, a weight 34, thereby polishing the workpiece 16.
  • the polishing pad 18 preferably has 54.3 to 65.1 volume percent pores, 34.9 to 45.7 volume percent PES resin, and a durometer hardness (Type-D) of 34.0 to 54.0.
  • the thin plate-shaped molded body that has undergone the precipitation process P3 is left for approximately five hours in warm water at a temperature higher than the cold water and the melting point of 2-pyrrolidone, for example, 40 to 60°C.
  • the drying process P5 the thin plate-shaped molded body is dried until all moisture is removed. This results in a thin plate-shaped PES resin or PVDF-HFP resin porous resin body (base resin of polishing pad 18) 17 with micropores of approximately 3 to 20 ⁇ m.
  • polishing test 1 The following describes polishing test 1 conducted by the inventors on semiconductor wafers.
  • comparative examples 1 and 2 and examples 1 to 5 shown in FIG. 6 were applied to an apparatus configured similarly to the surface polishing apparatus 10 shown in FIG. 1, and 4-inch diameter SiC wafers were polished under the test conditions for polishing test 1 described below.
  • Examples 1 to 4 were produced using the manufacturing process shown in FIG. 3, with different ratios of PES resin to 2-pyrrolidone.
  • FIG. 7 shows the volume fraction of PES resin, volume fraction of pores, and durometer hardness (Type-D) for Examples 1 to 4.
  • FIG. 8 shows an SEM photograph of example 3, which is representative of examples 1 to 5.
  • Comparative example 1 was composed of a rigid polyurethane resin in which pores of 20 to 40 ⁇ m were formed using a pore-forming agent.
  • FIG. 9 shows an SEM photograph of comparative example 1. Pores of about 20 to 40 ⁇ m can be observed in the SEM photograph in Figure 9.
  • Comparative Example 2 is a nonwoven fabric in which intertwined polyester fibers are bonded with polyurethane resin, with gaps of about 100 ⁇ m formed between the fibers.
  • Figure 10 shows an SEM photograph of Comparative Example 2. Large pores of about 100 ⁇ m can be observed in the SEM photograph in Figure 10.
  • polishing rate PR surface roughness Sa
  • number of scratches on the SiC wafer after polishing test 1 and polishing test 2 described below.
  • polishing Rate PR Method for Measuring Polishing Rate PR
  • the difference in mass of the SiC wafer before and after the polishing test was determined using an analytical balance, and the polishing amount (wear thickness) was determined from the known density of the SiC wafer and the surface area of the polished surface.
  • the polishing rate PR (nm/h) was calculated by dividing the polishing amount by the polishing time.
  • Figure 6 shows the polishing test results (polishing rate PR (nm/h) and surface roughness Sa (nm) of the polished surface) for Examples 1-5 and Comparative Examples 1-2.
  • the polishing results show that Examples 1-5 achieved a higher polishing rate PR (nm/h) than Comparative Examples 1-2. Furthermore, Examples 1-5 achieved a better surface roughness Sa than Comparative Examples 1-2.
  • SiC wafers are polished while supported by the edges of the bubbles, but because Examples 1-5 have minute pores, they are supported by many edges, which is thought to be the reason for the above polishing results.
  • Example product 3 in Figure 7 was applied to an apparatus configured similarly to surface polishing apparatus 10 shown in Figure 1, and a 4-inch ⁇ SiC wafer was polished under the same test conditions as those in Polishing Test 1 except for the polishing time.
  • the polishing rate PR (nm/h), the surface roughness Sa (nm) of the polished surface, and the number of scratches (count) were measured 22 times every time the polishing time elapsed until 200 hours had elapsed.
  • Figure 11 shows the polishing rate PR (nm/h), surface roughness Sa (nm) of the polished surface, and number of scratches (count) obtained from the 22 measurements.
  • Figure 12 is a line graph showing the change in polishing rate PR during polishing of a SiC wafer.
  • Figure 13 is a line graph showing the change in surface roughness Sa during polishing of a SiC wafer.
  • Figure 14 is a line graph showing the change in the number of scratches during polishing of a SiC wafer.
  • circles indicate values for Example Product 3
  • triangles indicate values for Comparative Example Product 1
  • squares indicate values for Comparative Example Product 2.
  • Example Product 3 exhibits a higher polishing rate PR than Comparative Product 1, while remaining at a roughly constant value.
  • the polishing rate PR of Comparative Product 2 was generally low and decreased over polishing time, with fuzzing occurring and chipping around the periphery of the pad after 70 hours, making polishing impossible.
  • the polyester fiber (non-woven fabric) of Comparative Product 2 is thought to have low resistance to strong oxidizing agents.
  • Example Product 3 exhibits a lower surface roughness Sa than Comparative Product 1, while remaining at a roughly constant value.
  • the surface roughness Sa of Comparative Product 1 varies periodically, while the surface roughness Sa of Comparative Product 2 increases over the polishing time, becoming unpolishable after 70 hours.
  • Example Product 3 has fewer scratches than Comparative Example Product 1, and the number remains constant (value "0").
  • the number of scratches on Comparative Example Product 1 shows a periodic increase, while the number of scratches on Comparative Example Product 2 increases over the polishing time, becoming unpolishable after 70 hours.
  • the porous resin body 17 of this embodiment uses a base resin of PES (polyethersulfone) resin or PVDF-HFP (a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene) resin, which has high resistance to oxidizing agents and abrasion, and the size of the micropores formed within the base resin is 2 to 20 ⁇ m.
  • PES polyethersulfone
  • PVDF-HFP a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene
  • a compound semiconductor polishing pad used in CMP polishing of difficult-to-polish wafers using a resin polishing pad that mechanically promotes polishing and a polishing solution that chemically promotes polishing, a compound semiconductor polishing pad that is free of scratches and can maintain its polishing rate and surface roughness for a long period of time can be obtained.
  • the porous resin body 17 of this embodiment has micropores measuring 2 to 20 ⁇ m in size. Therefore, when the polishing pad 18 incorporating this porous resin body 17 is used to polish hard-to-polish compound semiconductor wafers by the CMP method using a polishing solution containing a strong permanganate-based oxidizing agent, it is free from scratches and can maintain the polishing rate and surface roughness for a long period of time.
  • the manufacturing method of the resin porous body 17 that constitutes the polishing pad 18 of this embodiment includes a melt preparation process P1 in which a base resin with high resistance to oxidizing agents and wear resistance is melted in a high-melting-point organic solvent that has a melting point at room temperature (10 to 30°C) and is soluble in water to obtain a melt; a molding process P2 in which the melt is molded into a thin plate to obtain a thin plate-like molded body; a precipitation process P3 in which the thin plate-like molded body is placed in cold water that is lower than the melting point of the high-melting-point organic solvent to finely precipitate the high-melting-point organic solvent in the thin plate-like molded body; a substitution process P4 in which the thin plate-like molded body that has undergone the precipitation process P3 is placed in warm water that is higher than the temperature of the cold water and the melting point of the high-melting-point organic solvent to replace the solid high-melting-point organic solvent that has finely
  • the base resin in this example is PES (polyethersulfone) resin or PVDF-HFP (a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene) resin, resulting in a porous resin body with high resistance to oxidizing agents and abrasion.
  • PES polyethersulfone
  • PVDF-HFP a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene
  • the high-melting-point organic solvent is 2-pyrrolidone, which has a melting point of 24.6°C, or DMSO (dimethyl sulfoxide), which has a melting point of 18.4°C.
  • the thin plate-shaped molded body is left in cold water whose temperature is lower than the melting point of the high-melting-point organic solvent, allowing the high-melting-point organic solvent to be finely precipitated as a solid within the thin plate-shaped molded body.
  • the precipitation step P3 involves leaving the thin plate-shaped body in cold water at 5 to 10°C
  • the substitution step P4 involves leaving the thin plate-shaped body that has undergone the precipitation step P3 in warm water at 40 to 60°C, which is sufficiently higher than the melting point of the high-melting-point organic solvent. This allows the high-melting-point organic solvent solid to be finely precipitated in the thin plate-shaped body, and then the high-melting-point organic solvent solid that has precipitated in the thin plate-shaped body is replaced with water in the warm water.
  • the porous resin body of this embodiment has micropores with an average diameter of 2 to 20 ⁇ m, preferably 2 to 10 ⁇ m. This has the advantage that when polishing the workpiece 16 with a polishing pad 18 made of a porous resin body, the edges of the numerous micropores contribute to the polishing mechanism, making scratches less likely to occur, and achieving an optimal polishing rate PR and surface roughness Sa.
  • the polishing pad 18 of this embodiment has 54.3 to 65.1 volume percent pores, 34.9 to 45.7 volume percent PES resin, and a durometer hardness of 34.0 to 54.0, so it is free from scratches and can maintain the polishing rate PR and surface roughness Sa for long periods of time.
  • the polishing pad 118 is composed of a porous resin body 117 containing minute pores with an average diameter of 0.2 to 3 ⁇ m.
  • the porous resin body 117 functions as the base resin of the polishing pad 118.
  • the porous resin body 117 is made of PES (polyethersulfone) resin, which does not contain abrasive grains, or PVDF-HFP resin (a copolymer resin composed of 80% polyvinylidene fluoride and 20% propylene hexafluoride), and is molded into a sheet approximately 2 to 3 mm thick.
  • PES resin and PVDF-HFP resin have high resistance to the strong oxidizing agent, permanganate, in the polishing solution PF, and abrasion resistance that allows for a high polishing rate PR.
  • the chemical structure of PES resin is shown in Figure 4, and the chemical structure of PVDF-HFP resin is shown in Figure 5.
  • the polishing pad 118 preferably has 48.4 to 85.2 volume percent porosity, 14.8 to 51.6 volume percent base resin, and a durometer hardness (Type-D) of 12.5 to 58.1.
  • the thin plate-like molded body is left in cold water at a temperature, for example, 5 to 10°C, which is sufficiently lower than the melting point of lactose (202.8°C), for about 5 hours, thereby causing fine precipitation of solid lactose in the thin plate-like molded body.
  • These fine lactose precipitates (crystals) form micropores in the PES resin after the drying step P5 described below. The size of these micropores is adjusted by the temperature of the cold water and the standing time, but an average diameter of 0.2 to 3 ⁇ m is preferred.
  • the thin plate-shaped molded body that has undergone the precipitation step P3 is left for approximately 5 hours in warm water at a temperature higher than that of the cold water and the melting point of 2-pyrrolidone, for example, 40 to 60°C.
  • This replaces the lactose solids that have precipitated finely in the thin plate-shaped molded body and the organic solvent in the thin plate-shaped molded body with water, and hardens the thin plate-shaped molded body.
  • the drying step P5 the thin plate-shaped molded body is dried until all moisture is removed. This results in a thin plate-shaped PES resin or PVDF-HFP resin porous resin body (base resin of the polishing pad 18) 17 with micropores of approximately 0.2 to 3 ⁇ m.
  • N - methyl-2-pyrrolidone has the chemical formula C5H9NO , a freezing point of -24°C and a boiling point of 202°C, is soluble in water, and is capable of dissolving the base resin (PES resin or PVDF-HFP resin).
  • PES resin base resin
  • PVDF-HFP resin polyvinyl-N
  • polishing test 3 The following describes polishing test 3 for semiconductor wafers conducted by the present inventors.
  • comparative examples 1 and 2 shown in FIG. 15 and example examples 11 to 15 were applied to an apparatus configured similarly to the surface polishing apparatus 10 shown in FIG. 1, and 4-inch diameter SiC wafers were polished under the test conditions for polishing test 3 described below.
  • Example examples 11 and 12 were produced using the manufacturing process shown in FIG. 3, with the proportions of N-methyl-2-pyrrolidone, lactose, and PES resin changed so that the resulting porosity (volume %) differed from example to example.
  • Example examples 13 and 14 were produced using the manufacturing process shown in FIG.
  • Figures 18 and 19 show SEM photographs at 500x and 10,000x magnification of Example Product 12, which is representative of Examples 11 to 14. Micropores of approximately 0.2 to 2 or 3 ⁇ m are observed in the SEM photograph of Figure 19.
  • Figures 20 and 21 show SEM photographs at 500x and 10,000x magnification of Example Product 15. Uniform micropores of approximately 0.2 to 3 ⁇ m are observed in the SEM photograph of Figure 21.
  • Example Product 15 uses 2-pyrrolidone, which has a melting point at room temperature (24.6°C), as the organic solvent to dissolve the base resin. Therefore, in the precipitation step P3, solid 2-pyrrolidone is precipitated in addition to lactose, contributing to the formation of pores.
  • DMSO dimethyl sulfoxide
  • DMSO dimethyl sulfoxide
  • polishing Rate PR Method for Measuring Polishing Rate PR
  • the difference in mass of the SiC wafer before and after the polishing test was determined using an analytical balance, and the polishing amount (wear thickness) was determined from the known density of the SiC wafer and the surface area of the polished surface.
  • the polishing rate PR (nm/h) was calculated by dividing the polishing amount by the polishing time.
  • Figure 15 shows the polishing test results (polishing rate PR (nm/h) and surface roughness Sa (nm) of the polished surface) for Examples 11-15 and Comparative Examples 1-2.
  • the polishing results show that Examples 11-15 achieved a higher polishing rate PR (nm/h) than Comparative Examples 1-2. Furthermore, Examples 11-15 achieved a better surface roughness Sa than Comparative Examples 1-2.
  • SiC wafers are polished while supported by the edges of the bubbles, but Example Products 11-15 have microscopic pores of approximately 0.2-3 ⁇ m, so the wafers are supported by many edges, which is thought to be the reason for the above polishing results.
  • the porous resin body 117 of this embodiment uses a base resin of PES (polyethersulfone) resin or PVDF-HFP (a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene) resin, which has high resistance to oxidizing agents and abrasion, and the size of the micropores formed within the base resin is 0.2 to 3 ⁇ m.
  • PES polyethersulfone
  • PVDF-HFP a copolymer of 80% polyvinylidene fluoride and 20% hexafluoropropylene
  • a compound semiconductor polishing pad used in CMP polishing of difficult-to-polish wafers using a CMP method, which uses a resin polishing pad that mechanically promotes polishing and a polishing solution that chemically promotes polishing, a compound semiconductor polishing pad that is free of scratches and can maintain its polishing rate and surface roughness for a long period of time can be obtained.
  • the manufacturing method of the resin porous body 117 that constitutes the polishing pad 118 of this embodiment includes a melt preparation process P1 in which a base resin and lactose that are highly resistant to oxidizing agents and abrasion are melted in an organic solvent to obtain a melt; a molding process P2 in which the melt is molded into a thin plate to obtain a thin plate-like molded body; a precipitation process P3 in which the thin plate-like molded body is left in cold water that is lower than the melting point of lactose to precipitate fine solid lactose in the thin plate-like molded body; a replacement process P4 in which the thin plate-like molded body that has undergone the precipitation process P3 is left in warm water that is higher in temperature than the cold water to replace the finely precipitated lactose solid in the thin plate-like molded body and the organic solvent in the thin plate-like molded body with water; and a drying process P5 in which the thin plate-like molded body is dried until all moisture is removed from

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Abstract

L'invention concerne un corps en résine poreux ayant des pores fins, un tampon de polissage de semi-conducteur composé et un procédé de fabrication du corps en résine poreux. Le procédé de fabrication du corps en résine poreux comprend : une étape de préparation de masse fondue P1 pour obtenir une masse fondue par fusion d'une résine de matériau de base dans un solvant organique à point de fusion élevé ayant un point de fusion à température ambiante ; une étape de moulage P2 pour obtenir un corps moulé en forme de plaque mince par moulage de la masse fondue en une forme de plaque mince ; une étape de précipitation P3 pour précipiter finement le solvant organique à point de fusion élevé dans le corps moulé en forme de plaque mince en laissant le corps moulé en forme de plaque mince dans de l'eau froide à une température inférieure au point de fusion du solvant organique à point de fusion élevé ; une étape de remplacement P4 pour remplacer le solvant organique solide à point de fusion élevé précipité dans le corps moulé en forme de plaque mince par de l'eau en laissant le corps moulé en forme de plaque mince qui a traversé l'étape de précipitation P3 dans de l'eau chaude à une température supérieure à la température de l'eau froide et au point de fusion du solvant organique à point de fusion élevé ; et une étape de séchage P5 pour sécher le corps moulé en forme de plaque mince jusqu'à ce que le corps moulé en forme de plaque mince soit exempt d'humidité.
PCT/JP2025/012613 2024-03-27 2025-03-27 Corps en résine poreux, tampon de polissage de semi-conducteur composé et procédé de fabrication de corps en résine poreux Pending WO2025206235A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP2024-052458 2024-03-27
JP2024052459A JP7637467B1 (ja) 2024-03-27 2024-03-27 樹脂多孔体、化合物半導体研磨パッド、樹脂多孔体の製造方法
JP2024-052459 2024-03-27
JP2024052458A JP7571326B1 (ja) 2024-03-27 2024-03-27 化合物半導体研磨パッド、及び樹脂多孔体の製造方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02208332A (ja) * 1989-02-08 1990-08-17 Asahi Chem Ind Co Ltd 高分子多孔体の製造方法
JP2000349053A (ja) * 1999-06-07 2000-12-15 Asahi Chem Ind Co Ltd 溝付研磨パッド
JP2001164029A (ja) * 1999-12-10 2001-06-19 Terumo Corp 多孔質膜およびその製造方法
WO2003099933A1 (fr) * 2002-05-29 2003-12-04 Daicel Chemical Industries, Ltd. Dispersion et procede de production de moulages utilisant une dispersion
JP2009274208A (ja) * 2002-05-23 2009-11-26 Cabot Microelectronics Corp 微小孔性研磨パッド
JP2011194508A (ja) * 2010-03-19 2011-10-06 Fujibo Holdings Inc 研磨パッド
WO2012036034A1 (fr) * 2010-09-14 2012-03-22 国立大学法人大阪大学 Milieu poreux de polyacrylonitrile modifié par une amidoxime
JP2016505363A (ja) * 2012-12-03 2016-02-25 ロッテ ケミカル コーポレーション 精密ろ過膜または限外ろ過膜製造用高分子樹脂組成物、高分子ろ過膜の製造方法および高分子ろ過膜
JP2016147966A (ja) * 2015-02-12 2016-08-18 三菱樹脂株式会社 多孔質フィルム
WO2017038898A1 (fr) * 2015-09-04 2017-03-09 東京応化工業株式会社 Film poreux et son procédé de production
WO2018021337A1 (fr) * 2016-07-25 2018-02-01 宇部興産株式会社 Film poreux de polyéther sulfone et son procédé de production
JP2018172524A (ja) * 2017-03-31 2018-11-08 東ソー株式会社 ネットワーク状高分子多孔質粒子の新規な製造方法
JP2021057368A (ja) * 2019-09-26 2021-04-08 株式会社ノリタケカンパニーリミテド 半導体ウェハの研磨方法
JP2022149241A (ja) * 2021-03-25 2022-10-06 株式会社ノリタケカンパニーリミテド 研磨パッド
JP2023061016A (ja) * 2021-10-19 2023-05-01 株式会社ノリタケカンパニーリミテド 研磨パッド及びその製造方法

Patent Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02208332A (ja) * 1989-02-08 1990-08-17 Asahi Chem Ind Co Ltd 高分子多孔体の製造方法
JP2000349053A (ja) * 1999-06-07 2000-12-15 Asahi Chem Ind Co Ltd 溝付研磨パッド
JP2001164029A (ja) * 1999-12-10 2001-06-19 Terumo Corp 多孔質膜およびその製造方法
JP2009274208A (ja) * 2002-05-23 2009-11-26 Cabot Microelectronics Corp 微小孔性研磨パッド
WO2003099933A1 (fr) * 2002-05-29 2003-12-04 Daicel Chemical Industries, Ltd. Dispersion et procede de production de moulages utilisant une dispersion
JP2011194508A (ja) * 2010-03-19 2011-10-06 Fujibo Holdings Inc 研磨パッド
WO2012036034A1 (fr) * 2010-09-14 2012-03-22 国立大学法人大阪大学 Milieu poreux de polyacrylonitrile modifié par une amidoxime
JP2016505363A (ja) * 2012-12-03 2016-02-25 ロッテ ケミカル コーポレーション 精密ろ過膜または限外ろ過膜製造用高分子樹脂組成物、高分子ろ過膜の製造方法および高分子ろ過膜
JP2016147966A (ja) * 2015-02-12 2016-08-18 三菱樹脂株式会社 多孔質フィルム
WO2017038898A1 (fr) * 2015-09-04 2017-03-09 東京応化工業株式会社 Film poreux et son procédé de production
WO2018021337A1 (fr) * 2016-07-25 2018-02-01 宇部興産株式会社 Film poreux de polyéther sulfone et son procédé de production
JP2018172524A (ja) * 2017-03-31 2018-11-08 東ソー株式会社 ネットワーク状高分子多孔質粒子の新規な製造方法
JP2021057368A (ja) * 2019-09-26 2021-04-08 株式会社ノリタケカンパニーリミテド 半導体ウェハの研磨方法
JP2022149241A (ja) * 2021-03-25 2022-10-06 株式会社ノリタケカンパニーリミテド 研磨パッド
JP2023061016A (ja) * 2021-10-19 2023-05-01 株式会社ノリタケカンパニーリミテド 研磨パッド及びその製造方法

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