专利摘要:
A method of forming a composite polishing layer of a chemical mechanical polishing pad is provided, comprising: providing a first polishing layer component of a first continuous non-fugitive polymeric phase having a plurality of cavities periodicals; discharging a combination towards the first polishing layer component at a speed of 5 to 1000 m / s, filling the plurality of periodic cavities with the combination; solidifying the combination in the plurality of periodic cavities forming a second non-fugitive polymeric phase giving a composite structure; and obtaining the composite polishing layer of a chemical mechanical polishing pad from the composite structure, wherein the composite polishing layer of a chemical mechanical polishing pad has a polishing surface on the side of polishing the first polishing layer component; and wherein the polishing surface is adapted to polish a substrate.
公开号:FR3037836A1
申请号:FR1655968
申请日:2016-06-27
公开日:2016-12-30
发明作者:Bainian Qian；Brufau Teresa Brugarolas；Julia Kozhukh；David Michael Veneziale；Yuhua Tong；Diego Lugo；George C Jacob；Jeffrey B Miller；Tony Quan Tran；Marc R Stack；Andrew Wank；Jeffrey James Hendron
申请人:Rohm and Haas Electronic Materials CMP Holdings Inc；Dow Global Technologies LLC；
IPC主号:

专利说明:

[0001] TECHNICAL FIELD The present invention relates to a method of forming a composite polishing layer of a chemical mechanical polishing pad. More particularly, the present invention relates to a method of forming a composite polishing layer of a chemical mechanical polishing pad using an axial mixing device. In the manufacture of integrated circuits and other electronic devices, multiple layers of conductive, semiconductor and dielectric materials on and removed from a surface of a semiconductor wafer. Thin conductive, semiconductor and dielectric thin layers deposited using a number of deposition. Conventional deposition techniques in the form of wafer materials can be modern wafer processing techniques include physical vapor deposition (PVD), also known as cathodic sputtering, chemical deposition in phase. Examples of common techniques include isotropic and anisotropic etching in the wet and dry state, among others. As layers of material are deposited and removed sequentially, the top surface of the wafer becomes non-planar As the subsequent semiconductor processing (eg, metallization) requires the wafer to have a flat surface, the wafer must be planarized. Planarization is useful for eliminating undesirable surface topography and surface defects such as rough surfaces, m agglomerates, crystal lattice damage, scratches and contaminated layers or materials. Mechano-chemical planarization or mechano-chemical polishing (CMP) is a common technique used to plan or polish workpieces such as semiconductor wafers. In a conventional CMP, a wafer carrier or a polishing head is mounted on a carrier assembly. The polishing head holds the wafer and places it in contact with a polishing layer of a polishing pad which is mounted on a table or tray in a CMP apparatus. The support assembly provides controllable pressure between the wafer and the polishing pad. At the same time, a polishing medium (e.g., suspension) is dispensed onto the polishing pad and is drawn into the gap between the wafer and the polishing layer. To polish, the polishing pad and the wafer usually rotate relative to each other. When the polishing pad rotates under the wafer, the wafer scans a usually annular polishing path or a polishing region in which the surface of the wafer is directly in front of the polishing layer. The surface of the slab is polished and planarized by the chemical and mechanical action of the polishing layer and the polishing medium on the surface.
[0002] James et al. describe the importance of grooving in the polishing surface of the mechano-chemical polishing pads in U.S. Patent No. 6,736,709. Specifically, James et al. indicate that the "Groove Stiffness Quotient" ("GSQ") evaluates the effects of grooving on the stiffness of the pad and the "Groove Flow Quotient" ("Groove Flow Quotient" ("Groove Flow Quotient") "GFQ")) evaluates the effects of grooving on the fluid flow (interface with the buffer), and that there is a delicate balance between GSQ and GFQ in choosing an ideal polishing surface for a given polishing process. Nevertheless, as the dimensions of the wafers continue to shrink, the demands for the associated polishing process are becoming increasingly important, therefore, there is a continuing need for polishing layer configuration that broadens the operational performance range. mechano-chemical polishing pads and methods of producing the same.
[0003] The present invention provides a method of forming a composite polishing layer of a chemical mechanical polishing pad, comprising: providing a first polishing layer component of the composite polishing layer of chemical mechanical polishing; wherein the first component of the polishing layer has a polishing side, a base surface, a plurality of periodic cavities and an average thickness of the first component, T1_ avg measured perpendicularly to the polishing side from the base surface to the polishing side; wherein the first component of the polishing layer comprises a first continuous non-fugitive polymeric phase; wherein the plurality of periodic cavities has an average cavity depth, Davg, measured perpendicularly to the polishing side from the polishing side turned towards the base surface, where the average cavity depth, Davg, is less than the average thickness of the first component, Ti_avg, where the first continuous non-fugitive polymeric phase is a reaction product of a continuous first phase isocyanate-terminated urethane prepolymer having 8 to 12 wt% NCO groups; unreacted and a first phase curing agent; providing a poly (P) side liquid component, comprising at least one of a side polyol (P), a side side polyamine (P) and an amine side alcohol (P); providing an iso (I) side liquid component comprising at least one polyfunctional isocyanate; the supply of a pressurized gas; providing an axial mixing device having an internal cylindrical chamber; wherein the inner cylindrical chamber has a closed end, an open end, an axis of symmetry, at least one side liquid supply port (P) which opens into the inner cylindrical chamber, at least one supply port in liquid side (I) which opens into the inner cylindrical chamber, and at least one tangential pressurized gas supply port which opens into the inner cylindrical chamber; where the closed end and the open end are perpendicular to the axis of symmetry; wherein the at least one side liquid supply port (P) and the at least one side liquid supply port (I) are disposed along a circumference of the inner cylindrical chamber near the closed end ; wherein the at least one tangential pressurized gas supply port is disposed along a circumference of the inner cylindrical chamber downstream of the at least one side liquid supply port (P) and the at least one supply port. in liquid side (I) from the closed end; wherein the poly-side liquid component (P) is introduced into the inner cylindrical chamber through the at least one side liquid supply port (P) at a side charge pressure (P) of 6,895 to 27,600 kPa ; wherein the side iso liquid component (I) is introduced into the inner cylindrical chamber through the at least one side liquid supply port (I) at a side load pressure (I) of 6,895 to 27,600 kPa; wherein a combined mass flow rate of the poly-side liquid component (P) and the iso-side liquid component (I) in the inner cylindrical chamber is from 1 to 500 g / s, such as, preferably, from 2 to 40 g / s or, more preferably, from 2 to 25 g / sec; wherein the poly-side liquid component (P), the iso-side liquid component (I) and the pressurized gas are mixed in the inner cylindrical chamber to form a combination; wherein the pressurized gas is introduced into the inner cylindrical chamber through the at least one tangential pressurized gas supply port with a supply pressure of 150 to 1500 kPa; wherein the rate of entry into the internal cylindrical chamber of the pressurized gas is 50 to 600 m / s calculated on the basis of perfect gas conditions at 20 ° C and a pressure of 1 atm, or preferably 75 at 350 m / s; evacuating the combination of the open end of the inner cylindrical chamber towards the polishing side of the first component of the polishing layer at a speed of 5 to 1000 m / s, or preferably 10 to 600 m / s or more preferably 15 to 450 m / s, filling the plurality of recess cavities with the combination; solidifying the combination as a second component of the polishing layer in the plurality of periodic cavities to form a composite structure; wherein the second component of the polishing layer is a second non-fugitive polymeric phase; and obtaining a chemical-mechanical polishing pad composite polishing layer from the composite structure, wherein the chemical-mechanical polishing pad composite polishing layer has a polishing surface on the polishing side of the first component of the polishing layer; and wherein the polishing surface is adapted to polish a substrate. According to a particular feature of the present invention, the method of the present invention further comprises: machining the composite structure to obtain the composite polishing layer of a chemical mechanical polishing pad; wherein the composite polishing layer of a chemical-mechanical polishing pad thus obtained has an average thickness of composite polishing layer, Tp_avg, measured perpendicular to the polishing surface from the base surface to the surface of polishing; wherein the average thickness of the first component, Ti-avg, equals the average thickness of the composite polishing layer, Tp_ avg; wherein the second non-fugitive polymeric phase occupying the plurality of periodic cavities has an average height, Havg, measured perpendicularly to the polishing surface from the base surface toward the polishing surface; and, where an absolute value of a difference, AS, between the average thickness of the composite polishing layer, Tp_avg, and the average height, Havg, is <0.5 μm.
[0004] According to another particular feature of the present invention, the method of the present invention further comprises: forming at least one groove in the polishing surface. According to another particular feature of the present invention, the provision of the first polishing layer component further comprises providing a mold having a bottom and a peripheral wall, wherein the bottom and the peripheral wall defining a mold cavity; providing a continuous first phase isocyanate-terminated urethane prepolymer having 8 to 12% by weight of unreacted NCO groups, continuous first phase curing agent and optionally, a plurality of hollow core polymeric materials; mixing the continuous first phase isocyanate-terminated urethane prepolymer and the first-phase continuous curing agent to form a mixture; pouring the mixture into the mold cavity; solidifying the mixture into a cake of the first continuous non-fugitive polymeric phase; obtaining a sheet from the cake; forming the plurality of periodic cavities in the sheet to provide the first polishing layer component.
[0005] According to a particular feature, the plurality of hollow core polymeric materials is incorporated in the first continuous non-fugitive polymeric phase at 1 to 58% by vol. According to another particular feature of the present invention, the poly (P) side liquid component comprises 25 to 95% by weight of a side polyol (P); wherein the side polyol (P) is a high molecular weight polyether polyol; wherein the high molecular weight polyether polyol has a number average molecular weight, MN, of 2,500 to 100,000 and an average of 4 to 8 hydroxyl groups per molecule. According to another particular feature of the present invention, the iso (I) side liquid component comprises a polyfunctional isocyanate having an average of two reactive isocyanate groups per molecule. According to another particular feature of the present invention, the pressurized gas is selected from the group consisting of CO2, N2, air and argon. According to another particular characteristic of the present invention, the internal cylindrical chamber has a circular cross section in a plane perpendicular to the axis of symmetry of the internal cylindrical chamber; wherein the open end of the inner cylindrical chamber has a circular opening perpendicular to the axis of symmetry of the inner cylindrical chamber; where the circular opening is concentric with the circular cross section; and wherein the circular aperture has an internal diameter of 2.5 to 6 mm.
[0006] According to another particular feature of the present invention, the polishing surface is adapted to polish a semiconductor wafer. The present invention provides a method of forming a composite polishing layer of a chemical mechanical polishing pad, comprising: providing a first polishing layer component of the composite polishing layer of chemical mechanical polishing pad ; wherein the first component of the polishing layer has a polishing side, a base surface, a plurality of periodic cavities and an average thickness of the first component, T1_ avg, measured perpendicular to the polishing side of the base surface polishing side; wherein the first component of the polishing layer comprises a first continuous non-fugitive polymeric phase; wherein the plurality of periodic cavities has an average cavity depth, Davg, measured perpendicularly to the polishing side from the polishing side turned towards the base surface, where the average cavity depth, Davg, is less than the average thickness of the first component, wherein the first continuous non-continuous polymeric phase is a reaction product of a continuous phase first isocyanate-terminated urethane prepolymer having 8 to 12% by weight of NCO groups having unreacted and a first phase curing agent; providing a poly (P) side liquid component comprising at least one side polyol (P), one side polyamine (P) and one side amine alcohol (P); providing an iso (I) side liquid component comprising at least one polyfunctional isocyanate; the supply of a pressurized gas; providing an axial mixing device having an internal cylindrical chamber; wherein the inner cylindrical chamber has a closed end, an open end, an axis of symmetry, at least one side liquid supply port (P) which opens into the inner cylindrical chamber, at least one port of a side liquid supply (I) which opens into the internal cylindrical chamber, and at least one tangential pressurized gas supply port which opens into the internal cylindrical chamber; where the closed end and the open end are perpendicular to the axis of symmetry; wherein the at least one side liquid supply port (P) and the at least one side liquid supply port (I) are disposed along a circumference of the inner cylindrical chamber near the closed end ; wherein the at least one tangential pressurized gas supply port is disposed along a circumference of the inner cylindrical chamber downstream of the at least one side liquid supply port (P) and the at least one supply port in liquid side (I) from the closed end; wherein the poly-side liquid component (P) is introduced into the inner cylindrical chamber through the at least one side liquid supply port (P) at a side charge pressure (P) of 6,895 to 27,600 kPa; wherein the iso-side liquid component (I) is introduced into the inner cylindrical chamber through the at least one side liquid supply port (I) at a side load pressure (I) of 6,895 to 27,600 kPa ; wherein a combined mass flow rate of the poly (P) side liquid component and the iso (I) side liquid component in the direction of the inner cylindrical chamber is from 1 to 500 g / s, such as, preferably from 2 to 9 g / s or, more preferably, 2 to 25 g / s; wherein the poly (P) side liquid component, the iso (I) side liquid component and the pressurized gas are mixed in the inner cylindrical chamber to form a combination; wherein the pressurized gas is introduced into the inner cylindrical chamber through the at least one tangential pressurized gas supply port with a supply pressure of 150 to 1500 kPa; wherein an inlet velocity in the internal cylindrical chamber of the pressurized gas is 50 to 600 m / s, calculated on the basis of perfect gas conditions at 20 ° C and a pressure of 1 atm, or preferably 75 at 350 m / s; removing the combination from the open end of the inner cylindrical chamber towards the polishing side of the first component of the polishing layer at a speed of 5 to 1000 m / s, or, preferably, at 600 m / s or, more preferably, from 15 to 450 m / s, filling the plurality of periodic cavities with the combination; solidifying the combination as a second component of the polishing layer in the plurality of periodic cavities to form a composite structure; wherein the second component of the polishing layer is a second non-fugitive polymeric phase; and machining the composite structure to obtain the composite polishing layer of chemical mechanical polishing pad; wherein the chemical-mechanical polishing pad composite polishing layer as obtained has an average thickness of composite polishing layer, Tp_avg, measured perpendicular to the polishing surface from the base surface to the surface of polishing; wherein the average thickness of the first component, Ti_avg, equals the average thickness of the composite polishing layer, Tp-avg, where the second non-fugitive polymeric phase occupying the plurality of periodic cavities has an average height, Havg, measured perpendicularly with respect to the polishing surface 35 from the base surface towards the polishing surface; where an absolute value of a difference, AS, between the average thickness of the composite polishing layer, TP-avgi 3037836 and the average height, Havg, is <0.5 μm; wherein the composite polishing layer of chemical mechanical polishing pad has a polishing surface on the polishing side of the first component of the polishing layer; and wherein the polishing surface is adapted to polish a substrate. The present invention provides a method of forming a composite polishing layer of a chemical mechanical polishing pad, comprising: providing a mold having a bottom and peripheral walls, wherein the bottom and the peripheral walls define a mold cavity; providing a continuous first phase isocyanate-terminated urethane prepolymer having 8 to 12% by weight of unreacted NCO groups, continuous first phase curing agent, and optionally, a plurality of polymeric hollow core materials; mixing the continuous first phase isocyanate-terminated urethane prepolymer, the first continuous phase curing agent and optionally the plurality of hollow core polymeric materials to form a mixture; pouring the mixture into the mold cavity; solidifying the mixture into a cake of a first continuous non-fugitive polymeric phase; obtaining a cake sheet; forming a plurality of periodic cavities in the sheet to provide a first polishing layer component of the composite chemical-mechanical polishing pad polishing layer; wherein the first polishing layer component has a polishing side, a base surface, a plurality of periodic recesses and an average thickness of the first component, T1-avg / measured perpendicular to the polishing side from the base surface to the polishing side; wherein the plurality of periodic cavities has an average cavity depth, Davg, measured perpendicular to the polishing side from the polishing side towards the base surface, where the average cavity depth, Davg, is less than average thickness of the first component, Ti-avg; providing a poly (P) side liquid component comprising at least one of a side polyol (P), a side polyamine (P) and an amine side alcohol (P); providing an iso (I) side liquid component comprising at least one polyfunctional isocyanate; supply of a pressurized gas; providing an axial mixing device having an internal cylindrical chamber; wherein the inner cylindrical chamber has a closed end, an open end, an axis of symmetry, at least one side liquid supply port (P) which opens into the inner cylindrical chamber, at least one orifice of a side liquid supply (I) which opens into the internal cylindrical chamber, and at least one tangential pressurized gas supply port which opens into the internal cylindrical chamber; where the closed end and the open end are perpendicular to the axis of symmetry; wherein the at least one side liquid supply port (P) and the at least one side liquid supply port (I) are disposed along a circumference of the inner cylindrical chamber near the closed end 20 ; wherein the at least one tangential pressurized gas supply port is disposed along a circumference of the inner cylindrical chamber downstream of the at least one side liquid supply port (P) and the at least one supply port. side liquid (I) from the closed end; wherein the poly-side liquid component (P) is introduced into the inner cylindrical chamber through the at least one side liquid supply port of (P) at a side load pressure (P) of 6,895 to 27,600 kPa; wherein the iso-side liquid component (I) is introduced into the inner cylindrical chamber through the at least one side liquid supply port (I) at a side charge pressure (I) of 6,895 to 27,600 kPa; wherein a combined mass flow rate of the poly-side liquid component (P) and the iso-side liquid component (I) in the inner cylindrical chamber 35 is from 1 to 500 g / s, such as, preferably, from 2 to 40 g / s or more preferably from 2 to 25 g / s; wherein the poly (P) side liquid component, the iso (I) 3037836 12 liquid component and the pressurized gas are mixed in the inner cylindrical chamber to form a combination; wherein the pressurized gas is introduced into the inner cylindrical chamber through the at least one tangential pressurized gas supply port with a supply pressure of 150 to 1500 kPa; where an inlet velocity in the internal cylindrical chamber of the pressurized gas is 50 to 600 m / s calculated on the basis of the perfect gas conditions at 20 ° C and a pressure of 1 atm, or preferably 75 at 350 m / s; venting the combination from the open end of the inner cylindrical chamber to the polishing side of the first component of the polishing layer at a speed of 5 to 1000 m / s, or preferably 10 to 600 m / s or more preferably 15 to 450 m / s, filling the plurality of periodic cavities with the combination; solidifying the combination as a second polishing layer in the plurality of periodic cavities to form a composite structure; wherein the second polishing layer component is a second non-fugitive polymeric phase; and obtaining the chemical-mechanical polishing pad composite polishing layer from the composite structure, wherein the chemical-mechanical polishing pad composite polishing layer has a polishing surface of the first polishing layer component; and wherein the polishing surface is adapted to polish a substrate. BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a representation of a perspective view of a mold.
[0007] Figure 2 is a representation of a perspective view of a first polishing layer component. Figure 3 is a representation of a perspective view of a composite polishing layer of chemical mechanical polishing pad.
[0008] Figure 4 is a representation of a top view of a first polishing layer component.
[0009] Figure 5 is a cross-sectional view along line AA of Figure 4. Figure 6 is a side view representation of an axial mixing device for use in the method of the present invention. . Figure 7 is a cross-sectional view along the line B-B of Figure 6. Figure 8 is a cross-sectional view taken along line C-C of Figure 6.
[0010] Figure 9 is a representation of a side view of a composite structure formed according to the method of the present invention. Figure 10 is a representation of a top view of a chemical mechanical polishing pad having a composite polishing pad of chemical mechanical polishing pad of the present invention. Fig. 11 is a cross-sectional view along the line AA-AA of Fig. 11. Fig. 12 is a representation of a top view of a chemical-mechanical polishing pad composite polishing layer of the present invention. invention. Fig. 13a is a cross-sectional view taken along the line BB-BB of Fig. 12. Fig. 13b is another sectional view along the line BB-BB of Fig. 12. Fig. 14 is a representation of a perspective view of a chemical mechanical polishing pad having a composite polishing layer of a chemical mechanical polishing pad and a window.
[0011] DETAILED DESCRIPTION Historically, the GSQ and GFQ values for a polishing surface of a given polishing layer provided a workable range for designing effective polishing layers. Surprisingly, the present invention provides a method of producing composite polishing layers which provides a way out of the previously established GSQ and GFQ stereotype parameters for polishing layers by decoupling the stiffness and suspension distribution performance of the design of the polishing layers; thus increasing the design range of 5 polishing layers to achieve balances that was inaccessible until now regarding polishing performance properties. The term "non-fugitive" as used herein and in the appended claims with reference to a polymeric phase means that the polymeric phase (e.g., the second non-fugitive polymeric phase) does not melt, dissolve It does not disintegrate or selectively deplete in any other way with respect to another polymer phase (e.g., the first continuous non-fugitive polymeric phase) present in the composite polishing layer. The term "substantially circular cross-section" as used herein and in the appended claims with reference to a mold cavity (20) means that the longest radius, rc, of the mold cavity (20) ) projected on the xy plane (28) from the central axis of the mold cavity, Caris, (22) to a vertical internal boundary (18) of a peripheral wall (15) is 20% longer than the shortest radius, rc, of the mold cavity (20) projected on the xy plane (28) from the central axis of the mold cavity, Caris, (22) to the vertical internal boundary (18) . (See Figure 1) The term "mold cavity" as used herein and in the appended claims means the volume defined by a base (12) and a vertical internal boundary (18) of a peripheral wall (15). (See Figure 1) The term "substantially perpendicular" as used herein and in the appended claims with reference to a first characteristic (e.g., a horizontal internal boundary, a vertical internal boundary) with respect to a second characteristic (e.g. an axis, an xy plane) means that the first characteristic is at an angle of 80 to 100 ° with respect to the second characteristic. The term "substantially perpendicular" as used herein and in the appended claims with respect to a first characteristic (e.g., a horizontal internal boundary, a vertical internal boundary) with respect to a second characteristic (e.g. an axis, a plane xy) means that the first characteristic is at an angle of 85 to 95 ° with respect to the second characteristic.
[0012] The term "average thickness of the first component, 711_ avg" as used herein and in the appended claims with reference to the first component of the polishing layer (32) having a polishing side (37) refers to the of the first component, T1, of the first component of the polishing layer (32) measured perpendicular to the polishing sides (37) from the polishing side (37) to the base surface ( 35) of the first component of the polishing layer. (See Figure 2)
[0013] The term "average thickness of the composite polishing layer, Tp-avg" as used herein and in the appended claims with reference to a composite polishing layer of a chemical mechanical polishing pad (90) having a polishing surface (95) means the average thickness of the polishing layer, Tp, of the chemical-mechanical polishing pad composite polishing layer (90) in a direction perpendicular to the polishing surface ( 95) from the polishing surface (95) to the lower surface (92) of the chemical-mechanical polishing pad composite polishing layer (90). (See Figure 3) The term "substantially circular cross section" as used herein and in the appended claims with reference to a composite polishing layer of a chemical mechanical polishing pad (90) means that the longest radius, rp, from the cross-section of the central axis (98) of the chemical-mechanical polishing pad composite layer (90) to the outer perimeter (110) of the polishing surface (95) of the The chemical-mechanical polishing pad composite polishing layer (90) is 20% longer than the shortest radius, rp, of the cross-section from the central axis (98) to the outer perimeter (110) of the polishing surface (95). (See Figure 3) The chemical-mechanical polishing pad composite polishing layer (90) of the present invention is preferably adapted to rotate about a central axis (98). Preferably, the polishing surface (95) of the chemical-mechanical polishing pad composite polishing layer (90) is in a plane (99) perpendicular to the central axis (98). Preferably, the chemical-mechanical polishing pad composite polishing layer (90) is adapted to rotate in a plane (99) which is at an angle, γ, of 85 to 95 ° with respect to the central axis ( 98), preferably 90 ° to the central axis (98). Preferably, the chemical-mechanical polishing pad composite polishing layer (90) has a polishing surface (95) that has a substantially circular cross-section perpendicular to the central axis (98). Preferably, the radius rp of the cross-section of the polishing surface (95) perpendicular to the central axis (98) varies from <20% for the cross-section, more preferably by 10% for the cross section. cross. (See Figure 3) The term "gel time" as used herein and in the appended claims with reference to a combination of a poly (P) side liquid component and a iso (I) side liquid component. formed in an axial mixing device of the present invention, denotes the total curing time for this combination, determined using a standard test method according to ASTM D3795-00a (Re-approved in 2006) (Standard Test Method for Thermal Flow, 35 Cure, and Behavior Properties of Pourable Thermosetting Materials by Torque Rheometer).
[0014] The term "polyurethane" as used herein and in the appended claims includes (a) polyurethanes formed from the reaction of (i) isocyanates and (ii) polyols (including diols); and (b) a polyurethane formed by the reaction of (i) isocyanates with (ii) polyols (including diols) and (iii) water, amines or a combination of water and water. amines. A method of forming a composite polishing layer of a chemical-mechanical polishing pad (90), comprising: providing a first component of the polishing layer (32) of the composite buffer polishing layer chemical mechanical polishing (90); wherein the first component of the polishing layer (32) has a polishing side (37), a base surface (35), a plurality of periodic cavities (40) and an average first component thickness, measured perpendicular to the at the polishing side (37) from the base surface (35) to the polishing side (37); wherein the first component of the polishing layer (32) comprises a first continuous non-fugitive polymeric phase (30); wherein the plurality of periodic cavities (40) has an average cavity depth, Davg, of the polishing side (37) measured perpendicular to the polishing side (37) from the polishing side (37) towards the base surface (35), where the average cavity depth, Davg, is less than the average thickness of the first component, T1-avg; wherein the first continuous non-fugitive polymeric phase (30) is a reaction product of a continuous phase first isocyanate-terminated urethane prepolymer having 8 to 12% by weight unreacted NCO groups and 30% a first phase curing agent; providing a poly (P) side liquid component comprising at least one side polyol (P), one side polyamine (P) and one side amine alcohol (P); providing an iso (I) side liquid component comprising at least one polyfunctional isocyanate; the supply of a pressurized gas; providing an axial mixing device (60) having a cylindrical inner chamber (65); wherein the cylindrical inner chamber (65) has a closed end (62), an open end (68), an axis of symmetry (70), at least one side liquid supply port (P) (75) which opens in the cylindrical inner chamber (65), at least one side liquid supply port (I) (80) which opens into the cylindrical inner chamber (65), and at least one tangential pressurized gas supply (preferably at least two) (85) which opens into the inner cylindrical chamber (65); wherein the closed end (62) and the open end (68) are perpendicular to the axis of symmetry (70); wherein the at least one side liquid supply port (P) (75) and the at least one side liquid supply port and the at least one side liquid supply port (I) (80). ) are arranged along a circumference of the inner cylindrical chamber (65) near the closed end (62); wherein the at least one (preferably at least two) tangential pressurized gas supply port (85) is disposed along a circumference (67) of the inner cylindrical chamber (65) downstream of the at least one port 20 of supplying side liquid (P) (75) and at least one side liquid supply port (I) (80) from the closed end (62); wherein the poly-side liquid component (P) is introduced into the inner cylindrical chamber (65) through the at least one supply port (75) at a side load pressure kPa; wherein the liquid side liquid side component (P) (p) of 6,895 to 27,600 iso (I) is introduced into the inner cylindrical chamber (65) through the at least one side liquid supply port ( I) (80) at a side load pressure (I) of 6,895 to 27,600 kPa; wherein a combined mass flow rate of the poly (P) side liquid component and the iso (I) side liquid component in the inner cylindrical chamber is from 1 to 500 g / s (preferably from 2 to 40 g / s more preferably from 2 to 25 g / s); wherein the poly-side liquid component (P), the iso-side liquid component (I) and the pressurized gas are mixed in the inner cylindrical chamber (65) to form a combination where the pressurized gas is introduced into the cylindrical chamber 3037836 (65) by the at least one (preferably at least two) tangential pressurized gas supply port (85) with a supply pressure of 150 to 1500 kPa; wherein an inlet velocity in the internal cylindrical chamber (65) of the pressurized gas is 50 to 600 m / s calculated on the basis of perfect gas conditions at 20 ° C and a pressure of 1 atm, or preferably from 75 to 350 m / s; discharging the combination of the open end (68) from the inner cylindrical chamber (65) towards the polishing side (37) of the first polishing layer component (32) at a speed of from 5 to 1,000 m / s, or preferably from 10 to 600 m / s or, more preferably, from 15 to 450 m / s, filling the plurality of periodic cavities (40) with the combination; solidifying the combination as the second component of the polishing layer (45) in the plurality of periodic cavities (40) to form a composite structure (58); wherein the second component of the polishing layer (45) is a second non-fugitive polymeric phase (50); and obtaining the chemical-mechanical polishing pad composite polishing layer (90) from the composite structure (58), wherein the chemical-mechanical polishing pad composite polishing layer (90) has a surface polishing (95) on the polishing side (37) of the first component of the polishing layer (32); and wherein the polishing surface (95) is adapted to polish a substrate. (See Figures 1-14). Preferably, the first non-fugitive continuous polymeric phase (30) comprises a reaction product of a continuous phase first isocyanate-terminated urethane prepolymer having 8-12% by weight unreacted NCO groups and a curing agent. More preferably, the first continuous non-fugitive polymeric phase (30) comprises a reaction product of a continuous phase first iocyanate-terminated urethane prepolymer having 8.75 to 12% by weight of NCO groups not having reacted and a first phase curing agent continues. More preferably, the first non-continuous, continuous polymeric phase (30) comprises a reaction product of a continuous phase first isocyanate-terminated urethane prepolymer having 9.0 to 9.25 wt% NCO groups. unreacted and a first phase curing agent.
[0015] Preferably, the first continuous non-fugitive polymeric phase (30) is the reaction product of a continuous first phase isocyanate-terminated urethane prepolymer having 8 to 12% by weight unreacted NCO groups and a first phase curing agent; wherein the first continuous isocyanate-terminated urethane prepolymer is obtained from the interaction of a continuous first phase polyisocyanate (preferably a diisocyanate) with a continuous first phase polyol; wherein the continuous first phase polyol is selected from the group consisting of diols, polyols, polyol diols, copolymers thereof and mixtures thereof. Preferably, the continuous first phase polyol is selected from the group consisting of polytetramethylene ether glycol (PTMEG); a mixture of PTMEG with polypropylene glycol (PPG); and mixtures thereof with low molecular weight diols (eg, 1,2-butanediol, 1,3-butanediol, 1,4-butanediol). Preferably, the first non-fugitive continuous polymeric phase (30) is the reaction product of a continuous phase first isocyanate-terminated urethane prepolymer having 8 to 12% by weight of unreacted NCO groups and a first phase curing agent; wherein the first continuous phase curing agent is a continuous first phase polyamine. Preferably, the continuous first phase polyamine is an aromatic polyamine. More preferably, the continuous first phase polyamine is an aromatic polyamine selected from the group consisting of 4,4'-methylene-bis-ochloroaniline (MbOCA), 4,4'-methylene-bis- (3-chloro) -2,6-diethylaniline) (MCDEA); dimethylthiotoluenediamine; trimethylene glycol di-p-aminobenzoate; polytetramethyleneoxide di-p-aminobenzoate; polytetramethyleneoxide mono-p-aminobenzoate; polypropylene-di-p-aminobenzoate; polypropylene oxide mono-p-aminobenzoate; 1,2-bis (2-aminophenylthio) ethane; 4,4'-methylene-bis-aniline; diethyltoluenediamine; 5-tert-butyl-2,4-toluenediamine; 3-tert-butyl-2,6-toluenediamine; 5-tert-amyl-2,4-toluenediamine; 3- tert-amyl-2,6-toluenediamine; 5-tert-amyl-2,4-chlorotoluenediamine; and 3-tert-amyl-2,6-chlorotoluenediamine. Most preferably, the first continuous phase polyamine is 4,4'-methylene bis-o-chloroaniline (MbOCA). Examples of commercially available PTMEG-based isocyanate-terminated urethane prepolymers include Imuthane prepolymers (available from COIM USA, Inc., such as PET-80A, PET-85A, PET-90A, PET-93A, PET-95A, PET-60D, PET-70D, PET-75D); Adiprene® prepolymers (available from Chemtura, such as LF 800A, LF 900A, LF 910A, LF 930A, LF 931A, LF 939A, LF 950A, LF 952A, LF 600D, LF 601D, LF 650D, LF 667, LF 700D. , LF750D, LF751D, LF752D, LF753D and L325); Andur® prepolymers (available from Anderson Development Company, such as 70APLF, 80APLF, 85APLF, 90APLF, 95APLF, 60DPLF, 70APLF, 75APLF). Preferably, the continuous first phase isocyanate-terminated urethane prepolymer used in the process of the present invention is a low free monomer-terminated isocyanate-terminated urethane prepolymer having less than 0.1% by weight of content. in free toluene diisocyanate monomer (TDI). Preferably, the first non-continuous polymeric continuous phase (30) can be provided in both porous and non-porous (i.e., unfilled) configurations. Preferably, the first non-fugitive continuous polymeric phase (30) has a density of 0.5 measured according to ASTM D1622. More preferably, the first continuous non-fugitive polymeric phase (30) has a density of 0.5 to 1.2 (even more preferably 0.55 to 1.1, most preferably 0, 6 to 0.95) measured according to ASTM D1622.
[0016] Preferably, the first continuous non-fugitive polymeric phase (30) has a Shore D hardness of 40 to 90 measured according to ASTM D2240. More preferably, the first non-reactive polymeric phase (30) has a Shore D hardness of 50 to 75 measured according to ASTM D2240. Most preferably, the first continuous non-fugitive polymeric phase (30) has a Shore D hardness of 55 to 70 measured according to ASTM D2240. Preferably, the first non-fugitive continuous polymeric phase (30) is porous. Preferably, the first non-fugitive continuous polymeric phase comprises a plurality of microelements. Preferably, the plurality of microelements is uniformly dispersed throughout the first non-fugitive continuous polymeric phase (30). Preferably, the plurality of microelements is selected from entrapped gas bubbles, hollow core polymeric materials, liquid filled hollow core polymeric materials, water soluble materials, and insoluble phase material (e.g. mineral oil). More preferably, the plurality of microelements is selected from entrapped gas bubbles and hollow core polymeric materials uniformly distributed throughout the first continuous non-fugitive polymeric phase (30). Preferably, the plurality of microelements has a weight average diameter of less than 150 μm (more preferably less than 50 μm, most preferably 10 to 50 μm). Preferably, the plurality of microelements comprises polymeric micro-balloons with polyacrylonitrile shell walls or a polyacrylonitrile copolymer (eg, Expancel® from Akzo Nobel). Preferably, the plurality of microelements is incorporated in the first non-fugitive continuous polymeric phase (30) at 0 to 58% by vol. porosity (more preferably 1 to 58 vol%, most preferably 10 to 35 vol% porosity).
[0017] Preferably, the first non-fugitive continuous polymeric phase (30) has an open cell porosity of <6% in vol. (More preferably 5% by vol., even more preferably 4% by volume, most preferably <3% by vol.). polishing layer (32) provided in the method of producing a composite polishing layer of a chemical-mechanical polishing pad (90) of the present invention has a first component thickness, T1, measured perpendicular to the polishing side (37) of the base surface (35) to the polishing side (37). Preferably, the first component of the polishing layer (32) has an average thickness of the first component, Ti_avg, measured perpendicular to the polishing side (37) of the base surface (35) at the polishing side (37). ). More preferably, the first component of the polishing layer (32) has an average thickness of the first component, Ti_w, g, of 20 to 150 mils ((thousandths of an inch) ( more preferably, from 30 to 125 mils (0.76 to 3.17 mm), most preferably from 40 to 120 mils (1.00 to 3.05 mm) (see Figures 2 and 4). -5).
[0018] Preferably, the first component of the polishing layer (32) has a plurality of periodic cavities (40) having a depth, D, measured perpendicularly to the polishing side (37) of the polishing surface (37) to the base area. Preferably, the plurality of periodic cavities (40) has a mean depth, Davg; where Davg. More preferably, the plurality of periodic cavities (40) has a mean depth, Davg; where Davg 0, 5 * Ti-avg (more preferably Davg <0.4 * T1_avg, most preferably Davg 0375 * Ti_w, g). (See Figures 4-5). Preferably, the plurality of periodic cavities (40) is selected from curved cavities, linear cavities and combinations thereof. Preferably, the first component of the polishing layer has a plurality of periodic cavities, where the plurality of periodic cavities is a group of at least two concentric cavities. Preferably, the at least two concentric cavities have an average cavity depth, Davg, of 0.38 mm (15 mil: 1 mil = 10-3 inch = 0.0254 mm) (preferably, 0.38 to 1 mm (15 to 40 mils), more preferably 25 to 35 mils (0.69 to 0.89 mm), most preferably 30 mils (0.76 mm), of 5 mils (preferably 5 to 150 mils), more preferably 0.25 to 2.54 mm (10 to 100 mils). most preferably 0.38 to 1.27 mm (15 to 50 mils) and a spacing of 0.25 mm (10 mils) (preferably 0.63 to 3.8 mm). (25 to 150 mils), more preferably 50 to 100 mils (1.27 to 2.54 mm), most preferably, 60 to 80 mils (1.52 to 2.03 mm). . Preferably, the at least two concentric cavities have a width and a spacing, the width and the spacing being equal. Preferably, the plurality of periodic cavities (40) may be selected from the group consisting of a plurality of periodic cavities not interconnected and a plurality of periodic cavities interconnected. Preferably, when the plurality of periodic cavities is a plurality of periodic cavities not interconnected, the second non-fugitive polymeric phase is a discontinuous second non-fugitive polymeric phase. Preferably, when the plurality of periodic cavities is a plurality of interconnected periodic cavities, the second phase used in the process of the present invention is internally cylindrical (65). Preferably, polymeric axial (60) a non-fugitive polymeric chamber chamber is a second continuous non-fugitive phase. Preferably, the internal cylindrical mixing device (65) has a closed end (62) and an open end (68). Preferably, the closed end (62) and the cylindrical perpendicular end of the open end (68) are each substantially at an axis of symmetry (70) of the chamber (65). More preferably, (62) and the open end (68) are internally closed substantially perpendicular to an axis of symmetry (70) of the inner cylindrical chamber (65). Most preferably, the closed end (62) and the open end (68) are each perpendicular to an axis of symmetry (70) of the inner cylindrical chamber (65). (See Figures 6-8).
[0019] Preferably, the axial mixing device (60) used in the method of the present invention has an inner cylindrical chamber (65) with an axis of symmetry (70), where the open end (68) has a circular opening ( 69). More preferably, the axial mixing device (60) used in the method of the present invention has an inner cylindrical chamber (65) with an axis of symmetry (70); wherein the open end (68) has a circular opening (69); and wherein the circular opening (69) is concentric with respect to the inner cylindrical chamber (65). Most preferably, the axial mixing device (60) used in the method of the present invention has an inner cylindrical chamber (65) with an axis of symmetry (70); wherein the open end (68) has a circular opening (69); wherein the circular aperture (69) is concentric with the inner cylindrical chamber (65); and wherein the circular opening (69) is perpendicular to the axis of symmetry (70) of the inner cylindrical chamber (65). Preferably, the circular aperture (69) has a diameter of 1 to 10 mm (more preferably 1.5 to 7.5 mm, more preferably 2 to 6 mm; between all, 2.5 to 3.5 mm). (See Figures 6-8). Preferably, the axial mixing device (60) used in the method of the present invention has at least one side liquid supply port (P) (75) which opens into the inner cylindrical chamber (65). . More preferably, the axial mixing device (60) used in the method of the present invention has at least two side liquid supply ports (P) (75) which open into the inner cylindrical chamber (65). ). Preferably, when the axial mixing device (60) used in the method of the present invention has at least two side liquid supply ports (P) (75) which open into the inner cylindrical chamber (65), the at least two side liquid supply ports (P) (75) are uniformly disposed along the circumference (67) of the inner cylindrical chamber (65). More preferably, when the axial mixing device (60) used in the method of the present invention has at least two side liquid supply ports (P) (75) which open into the internal cylindrical chamber (65), the at least two side liquid supply ports (P) (75) are uniformly disposed along a circumference (67) of the inner cylindrical chamber (65) and are equidistant from the closed end (62) of the inner cylindrical chamber (65). Preferably, the at least one side liquid supply port (P) opens into the inner cylindrical chamber (65) through an orifice having an inner diameter of 0.05 to 3 mm (preferably 0 1 to 0.1 mm, more preferably 0.15 to 0.5 mm). Preferably, the at least one side liquid supply port (P) opens into the inner cylindrical chamber (65) and is directed toward the symmetry axis (70) of the inner cylindrical chamber (65). . More preferably, the at least one side liquid supply port (P) opens into the inner cylindrical chamber (65) and is directed towards and substantially perpendicular to the axis of symmetry (70) of the inner cylindrical chamber (65). Most preferably, the at least one side liquid supply port (P) opens into the inner cylindrical chamber (65) and is directed toward and perpendicular to the axis of symmetry (70) of the inner cylindrical chamber (65).
[0020] Preferably, the axial mixing device (60) used in the method of the present invention has at least one side liquid supply port (I) (80) which opens into the inner cylindrical chamber (65). . More preferably, the axial mixing device (60) used in the method of the present invention has at least two side liquid supply ports (I) (80) which open into the internal cylindrical chamber ( 65). Preferably, when the axial mixing device (60) used in the method of the present invention has at least two side liquid supply ports (I) (80) which open into the inner cylindrical chamber ( 65), the at least two side liquid supply ports (I) (80) are uniformly disposed along a circumference (67) of the inner cylindrical chamber (65). More preferably, when the axial mixing device (60) used in the method of the present invention has at least two side liquid supply ports (I) (80) which open into the internal cylindrical chamber (65), the at least two side liquid supply ports (I) (80) are uniformly disposed along a circumference (67) of the inner cylindrical chamber (65) and are equidistant from the end closed (62) of the inner cylindrical chamber (65). Preferably, the at least one side liquid supply port (I) opens into the inner cylindrical chamber (65) through an orifice having an internal diameter of 0.05 to 3 mm (preferably 0, 1 to 0.1 mm, more preferably 0.15 to 0.5 mm). Preferably, the at least one side liquid supply port (I) opens into the inner cylindrical chamber (65) through an orifice having an inner diameter of 0.05 to 1 mm (preferably 0, 1 to 0.75 mm, more preferably 0.15 to 0.5 mm). Preferably, the at least one side liquid supply port (I) opens into the inner cylindrical chamber (65) and is directed toward the axis of symmetry (70) of the inner cylindrical chamber (65). . More preferably, the at least one (I) side liquid supply port opens into the inner cylindrical chamber (65) and is directed towards and substantially perpendicular to the axis of symmetry (70). of the inner cylindrical chamber (65). Most preferably, the at least one side liquid supply port (I) opens into the inner cylindrical chamber (65) and is directed toward and perpendicular to the axis of symmetry (70). of the inner cylindrical chamber (65).
[0021] Preferably, the axial mixing device (60) used in the method of the present invention has at least one side liquid supply port (P) (75) which opens into the inner cylindrical chamber (65). ) and at least one side liquid supply port (I) (80) which opens into the inner cylindrical chamber (65); wherein the at least one side liquid supply port (P) (75) and the at least one side liquid supply port (I) (80) are disposed uniformly along the circumference (67) of the internal cylindrical chamber (65). More preferably, the axial mixing device (60) used in the method of the present invention has at least one side liquid supply (P) (75) which opens internal cylindrical chamber (65) and at least one A liquid supply side (I) (80) which opens internal cylindrical chamber (65); wherein the at least one in the orifice in the orifice in the side liquid supply port (P) (75) and the at least one side liquid supply port (I) (80) are arranged uniformly following a circumference (67) of the inner cylindrical chamber (65) and are equidistant from the closed end (62) of the inner cylindrical chamber (65). Preferably, the axial mixing device (60) used in the method of the present invention has at least two side liquid supply ports (P) (75) which open into the inner cylindrical chamber (65). and at least two side liquid supply ports (I) (80) which open into the inner cylindrical chamber (65). Preferably, when the axial mixing device (60) used in the method of the present invention has at least two side liquid supply ports (P) (75) which open into the internal cylindrical chamber (65). ) and at least two side liquid supply ports (I) (80) which open into the inner cylindrical chamber (65), the at least two side liquid supply ports (P) (75). ) are arranged uniformly along a circumference (67) of the inner cylindrical chamber (65) and the at least two side liquid supply ports (I) (80) are arranged uniformly along a circumference (67) of the internal cylindrical chamber (65). Preferably, when the axial mixing device (60) used in the process of the present invention has at least two side liquid supply ports (P) (75) which open into the inner cylindrical chamber (65). ) and at least two side liquid supply ports (I) (80) which open into the inner cylindrical chamber (65), the side liquid supply ports (P) (75) and the fluid supply ports (I) (80) alternate along a circumference (67) of the inner cylindrical chamber (65). More preferably, when the axial mixing device (60) used in the method of the present invention has at least two side liquid supply ports (P) (75) which open into the internal cylindrical chamber (65) and at least two side liquid supply ports (I) (80) which open into the inner cylindrical chamber (65), the side liquid supply ports (P) (75). and the side liquid supply ports (I) (80) alternate and are uniformly spaced along a circumference (67) of the inner cylindrical chamber (65). Most preferably, when the axial mixing device (60) used in the method of the present invention has at least two side liquid supply ports (P) (75) which open into the cylindrical chamber internal (65) and at least two side liquid supply ports (I) (80) which open into the inner cylindrical chamber (65); the side liquid supply ports (P) (75) and the side liquid supply ports (I) (80) alternate and are uniformly spaced along a circumference (67) of the internal cylindrical chamber (65). ); and the side liquid supply ports (P) (75) and the side liquid supply ports (I) (80) are all equidistant from the closed end (62) of the chamber internal cylindrical (65).
[0022] Preferably, the axial mixing device (60) used in the method of the present invention has at least one tangential pressurized gas supply port (85) which opens into the inner cylindrical chamber (65). More preferably, the axial mixing device (60) used in the method of the present invention has at least one tangential pressurized gas supply port (85) which opens into the inner cylindrical chamber (65); wherein the at least one tangential pressurized gas supply port (85) is disposed along a circumference of the inner cylindrical chamber (65) downstream of the at least one side liquid supply port (P) (75) and at least one side liquid supply port (I) (80) from the closed end (62). Even more preferably, the axial mixing device (60) used in the method of the present invention has at least two tangential pressurized gas supply ports (85) which open into the inner cylindrical chamber (65). ; wherein the at least two tangential pressurized gas supply ports (85) are disposed circumferentially of the inner cylindrical chamber (65) downstream of the at least one side liquid supply port (P) (75). and at least one side liquid supply port (I) (80) from the closed end (62). Even more preferably, the axial mixing device (60) used in the process of the present invention has at least two tangential pressurized gas supply ports (85) which open into the inner cylindrical chamber (65). ; wherein the at least two tangential pressurized gas supply ports (85) are disposed circumferentially of the inner cylindrical chamber (65) downstream of the at least one side liquid supply port (P) (75) and at least one side liquid supply port (I) (80) from the closed end (62); and wherein the at least two tangential pressurized gas supply ports (85) are uniformly disposed along a circumference (67) of the inner cylindrical chamber (65). Most preferably, the axial mixing device (60) used in the process of the present invention has at least two tangential pressurized gas supply ports (85) which open into the internal cylindrical chamber (65). ); wherein the at least two tangential pressurized gas supply ports (85) are disposed along the circumference of the inner cylindrical chamber (65) downstream of the at least one side liquid supply port (P) (75). and at least one side liquid supply port (I) (80) from the closed end (62); and wherein the at least two tangential pressurized gas supply ports (85) are uniformly disposed along a circumference (67) of the inner cylindrical chamber (65) and equidistant from the closed end (62) of the chamber internal cylindrical 15 (65). Preferably, the at least one tangential pressurized gas supply port opens into the inner cylindrical chamber (65) through an orifice having a critical dimension of 0.1 to 5 mm (preferably 0.3 to 3 mm). more preferably 0.5 to 2 mm). Preferably, the at least one tangential pressurized gas supply port opens into the inner cylindrical chamber (65) and is directed tangentially along an inner circumference of the inner cylindrical chamber (65). More preferably, the at least one tangential pressurized gas supply port opens into the inner cylindrical chamber (65) and is directed tangentially along an inner circumference of the inner cylindrical chamber and on a substantially perpendicular plane. to the axis of symmetry (70) of the inner cylindrical chamber (65). Most preferably, the at least one tangential pressurized gas supply port opens into the inner cylindrical chamber (65) and is directed tangentially along an inner circumference of the inner cylindrical chamber and on a plane which is perpendicular to the axis of symmetry (70) of the inner cylindrical chamber (65).
[0023] Preferably, in the process of the present invention, the poly (P) side liquid component comprises at least one of a side polyol (P), a side polyamine (P) and an amine alcohol side. (P).
[0024] Preferably, the side polyol (P) is selected from the group consisting of diols, polyols, polyol diols, copolymers thereof and mixtures thereof. More preferably, the side polyol (P) is selected from the group consisting of polyether polyols (e.g., poly (oxytetramethylene) glycol, poly (oxypropylene) glycol and mixtures thereof); polycarbonate polyols; polyester polyols; polycaprolactone polyols; mixtures thereof and mixtures thereof with one or more low molecular weight polyols selected from the group consisting of ethylene glycol; 1,2-propylene glycol; 1,3-propylene glycol; 1,2-butanediol; 1,3-butanediol; 2-methyl-1,3-propanediol; 1,4-butanediol; neopentyl glycol; 1,5-pentanediol; 3-methyl-1,5-pentanediol; 1,6-hexanediol; diethylene glycol; dipropylene glycol; and tripropylene glycol. Even more preferably, the at least one side polyol (P) is selected from the group consisting of polytetramethylene ether glycol (PTMEG); ester-based polyols (such as ethylene adipates, butylene adipates); polypropylene ether glycols (PPG); polycaprolactone polyols; their copolymers and their mixtures. Preferably, in the process of the present invention, the poly (P) side liquid component used contains at least one side polyol (P); wherein the at least one side polyol (P) comprises a high molecular weight polyol having a number average molecular weight, MN, of 2,500 to 100,000. More preferably, the high molecular weight polyol has a number average molecular weight, MN, from 5,000 to 50,000 (even more preferably from 7,500 to 25,000, most preferably from 10,000 to 12,000).
[0025] Preferably, in the process of the present invention, the poly (P) side liquid component used contains at least one side polyol (P); wherein the at least one side polyol (P) comprises a high molecular weight polyol having an average of three to ten hydroxyl groups per molecule. More preferably, the high molecular weight polyol used has an average of four to eight (even more preferably, five to seven, most preferably six) hydroxyl groups per molecule.
[0026] Examples of commercially available high molecular weight polyols include Specflex® polyols, Voranol® polyols, and Voralux® polyols (available from The Dow Chemical Company); Multranol® specialty polyols and Ultracelc flexible polyols (available from Bayer MaterialScience LLC); and Pluracol® polyols (available from BASF). Several preferred high molecular weight polyols are shown in TABLE 1.
[0027] TABLE 1 Polyol of High Molecular Weight Number of Groups MN Number of Hydroxyl Groups (mq KOH / q) OH per molecule Multranol® 3901 Polyol 3.0 6,000 28 Pluracol® 1385 Polyol 3.0 3 200 50 Pluracol® 380 Polyol 3 , 0 6 500 25 Pluracol® 1123 Polyol 3.0 7000 24 ULTRACEL® 3000 Polyol 4.0 7 500 30 SPECFLEX® NC630 Polyol 4.2 7 602 31 SPECFLEX® NC632 Polyol 4.7 8 225 32 VORALUX® HF 505 Polyol Preferably, the polyamine (P) is selected from the group consisting of diamines and other polyamines. multifunctional amines. More preferably, the side polyamine (P) is selected from the group consisting of aromatic diamines and other multifunctional aromatic amines such as, for example, 4,4'-methylene-bis-o-chloroaniline (&quot; MbOCA "); 4,4'-methylenebis- (3-chloro-2,6-diethylaniline) ("MCDEA"); dimethylthiotoluenediamine; trimethylene glycol di-p-aminobenzoate; polytetramethyleneoxide di-p-aminobenzoate; polytetramethyleneoxide mono-p-aminobenzoate; polypropylene oxide di-p-aminobenzoate; polypropylene oxide mono-p-aminobenzoate; 1,2-bis (2-aminophenylthio) ethane; 4,4'-methylene-bis-aniline; diethyltoluenediamine; 5- tert-butyl-2,4-toluenediamine; 3-tert-butyl-2,6-toluenediamine; 5-tert-amyl-2,4-toluenediamine; and 3-tert-amyl-2,6-toluenediamine and chlorotoluenediamine. Preferably, the side amine alcohol (P) is selected from the group consisting of amine initiator polyols. More preferably, the side amine alcohol (P) is selected from the group consisting of amine initiator polyols containing one to four (even more preferably, two to four, most preferably two) atoms. of nitrogen per molecule. Preferably, the amine side alcohol (P) is selected from the group consisting of amine initiator polyols which have on average at least three hydroxyl groups per molecule. More preferably, the amine side alcohol (P) is selected from the group consisting of amine initiator polyols which average from three to six (more preferably from three to five, most preferably four) hydroxyl groups per molecule. Particularly preferred amine initiator polyols have a number average molecular weight of 700 (preferably 150 to 650, more preferably 200 to 500, most preferably 250 to 300), and have a hydroxyl number (determined by the test method ASTM Test Method D4274-11) of 350 to 1200 mg KOH / g. More preferably, the amine-initiated polyol used has a hydroxyl number of 400 to 1000 mg KOH / g (most preferably 600 to 850 mg KOH / g). Examples of commercially available amine initiator polyols include the Voranol® amine initiator polyol family (available from The Dow Chemical Company); Quadrol® specialty polyols (N, N, N ', N'-tetrakis (2-hydroxypropylethylenediamine)) (available from BASF); Pluracol® amine-based polyols (available from BASF); Multranol® amine-based polyols (available from Bayer MaterialScience LLC); triisopropanolamine (TIPA) (available from The Dow Chemical Company); and triethanolamine (TEA) (available from Mallinckrodt Baker Inc.). Several preferred amine initiator polyols are shown in TABLE 2. TABLE 2 Amine-Initiated Polyol OH Groups OH Groups Hydroxyl Groups (mq KOH / q) Molecule Triethanolamine 3 149 1 130 Triisopropanolamine 3 192 877 MULTRANOL® 9138 Polyol 3 240 700 MULTRANOL® 9170 Polyol 3 481 350 VORANOL® 391 Polyol 4 568 391 VORANOL® 640 Polyol 4 352 638 VORANOL® 800 Polyol 4 280 801 QUADROL® Polyol 4 292 770 MULTRANOL® 4050 Polyol 4 356 630 MULTRANOL® 4063 Polyol 4 488 460 MULTRANOL® 8114 Polyol 4 568 395 MULTRANOL® 8120 Polyol 4 623 360 MULTRANOL® 9181 Polyol 4 291 770 VORANOL® 202 Polyol 5 590 475 20 3037836 36 Preferably, in the process of the present invention, the poly-side liquid component (P) is introduced into the inner cylindrical chamber (65) through the at least one side liquid supply port (P) (75) at a side load pressure (P) of 6,895 to 27,600 kPa . More preferably, the poly-side liquid component (P) is introduced into the inner cylindrical chamber (65) through the at least one side liquid supply port (P) (75) at a side load pressure. (P) from 8,000 to 20,000 kPa. Most preferably, the poly-side liquid component (P) is introduced into the inner cylindrical chamber (65) through the at least one side liquid supply port (P) (75) at a load pressure. side (P) of 10,000 to 17,000 kPa.
[0028] Preferably, in the process of the present invention, the iso (I) side liquid component comprises at least one polyfunctional isocyanate. Preferably, the at least one polyfunctional isocyanate contains two reactive isocyanate groups (ie, NCO).
[0029] Preferably, the at least one polyfunctional isocyanate is selected from the group consisting of a polyfunctional aliphatic isocyanate, a polyfunctional aromatic isocyanate and a mixture thereof. More preferably, the polyfunctional isocyanate is a diisocyanate selected from the group consisting of 2,4-toluene diisocyanate; 2,6-toluene diisocyanate; 4,4'-diphenylmethane diisocyanate; naphthalene-1,5-diisoc yanate; tolidine diisocyanate; para-phenylene diisocyanate; xylylene diisocyanate of isophorone diisocyanate; hexamethylene diisocyanate; 4,4'-dicyclohexylmethane diisocyanate; cyclohexanediisocyanate; and their mixtures. Still further polyfunctional isocyanate is isocyanate-terminated with a prepolymer polyol. Preferably, the at least one, at least one urethane prepolymer at the reaction of a diisocyanate is a polyfunctional isocyanate is an isocyanate-terminated urethane prepolymer; wherein the isocyanate-terminated urethane prepolymer has 2 to 12% by weight of unreacted isocyanate groups (NC0). More preferably, the isocyanate-terminated urethane prepolymer used in the process of the present invention has 2 to 10% by weight (even more preferably 4 to 8% by weight, most preferably 5 to 10% by weight). to 7% by weight) of unreacted isocyanate groups (NCO). Preferably, the isocyanate-terminated urethane prepolymer used is the reaction product of a diisocyanate with a prepolymer polyol; wherein the prepolymer polyol is selected from the group consisting of diols, polyols, polyol diols, their copolymers and mixtures thereof. More preferably, the polyol prepolymer is selected from the group consisting of polyether polyols (e.g., poly (oxytetramethylene) glycol, poly (oxypropylene) glycol, and mixtures thereof); polycarbonate polyols; polyester polyols; polycaprolactone polyols; mixtures thereof and mixtures thereof with one or more low molecular weight polyols selected from the group consisting of ethylene glycol; 1,2-propylene glycol; 1,3-propylene glycol; 1,2-butanediol; 1,3-butanediol; 2-methyl-1,3-propanediol; 1,4-butanediol; neopentyl glycol; 1,5-pentanediol; 3-methyl-1,5-pentanediol; 1,6-hexanediol; diethylene glycol; dipropylene glycol; and tripropylene glycol. Even more preferably, the prepolymer polyol is selected from the group consisting of polytetramethylene ether glycol (PTMEG); ester-based polyols (such as ethylene adipates, butylene adipates); polypropylene ether glycols (PPG); polycaprolactone polyols; of their copolymers; and their mixtures. Most preferably, the prepolymer polyol is selected from the group consisting of PTMEG and PPG. Preferably, when the prepolymer polyol is PTMEG, the isocyanate-terminated urethane prepolymer has a concentration of isocyanate groups which are not Reacted (NCO) from 2 to 10% by weight (more preferably from 4 to 8% by weight, most preferably from 6 to 7% by weight). Examples of commercially available PTMEG-based isocyanate-terminated urethane prepolymers include Imuthane prepolymers (available from COIM USA, Inc., such as PET-80A, PET-85A, PET-90A, PET-93A PET-95A, PET-60D, PET-70D, PET-75D); Adiprene® prepolymers (available from Chemtura, such as, LF 800A, LF 900A, LF 910A, LF 930A, LF 931A, LF 939A, LF 10 950A, LF 952A, LF 600D, LF 601D, LF 650D, LF 667, LF 700D, LF750D, LF751D, LF752D, LF753D and L325); Andur® prepolymers (available from Anderson Development Company, such as 70APLF, 80APLF, 85APLF, 90APLF, 95APLF, 60DPLF, 70APLF, 75APLF).
[0030] Preferably, when the prepolymer polyol is PPG, the isocyanate-terminated urethane prepolymer has an unreacted isocyanate group (NCO) concentration of 3 to 9% by weight (more preferably 4 to 10% by weight). 8% by weight, most preferably 5 to 6% by weight).
[0031] Examples of commercially available PPG-based isocyanate-terminated urethane prepolymers include Imuthane® prepolymers (available from COIM USA, Inc., such as PPT-80A, PPT-90A, PPT-95A, PPT- 65D, PPT-75D); Adiprene® prepolymers (available from Chemtura, such as LFG 963A, LFG 964A, LFG 740D); and Andur® prepolymers (available from Anderson Development Company, such as 8000APLF, 9500APLF, 6500DPLF, 7501DPLF). Preferably, the isocyanate-terminated urethane prepolymer used in the process of the present invention is a low monomer free isocyanate-terminated urethane prepolymer having less than 0.1% by weight of toluene monomer content. diisocyanate (TDI) free. The non-TDI-based isocyanate-terminated urethane prepolymers may also be used in the process of the present invention. For example, isocyanate-terminated urethane prepolymers include those formed by the reaction of 4,4'-diphenylmethane diisocyanate (MDI) and polyols such as polytetramethylene glycol (PTMEG) with optional diols such as 1, 4-butanediol (BDO) are acceptable. When these isocyanate-terminated urethane prepolymers are used, the concentration of unreacted isocyanate groups (NCO) is preferably from 4 to 10% by weight (more preferably from 4 to 8% by weight, most preferably 5 to 7% by weight). Examples of commercially available isocyanate-terminated urethane prepolymers in this class include Imuthane® prepolymers (available from COIM USA, Inc. such as 27-85A, 27-90A, 27-95A); Andur® prepolymers (available from Anderson Development Company, such as IE75AP, IE80AP, IE85AP, IE90AP, IE95AP, IE98AP); Vibrathane® prepolymers (available from Chemtura, such as B625, B635, B821); Isonate modified prepolymers (available from The Dow Chemical Company, such as Isonate! 240 with 18.7% NCO, Isonate 181 with 23% NCO, Isonate 143L with 29.2% NCO); and polymeric MDI (available from The Dow Chemical Company, such as PAPI '20, 27, 94, 95, 580N, 901). Preferably, in the process of the present invention, the iso-side liquid component (I) is introduced into the inner cylindrical chamber (65) through the at least one side liquid supply port (I) (80) to a side load pressure (I) of 6,895 to 27,600 kPa. More preferably, the iso-side liquid component (I) is introduced into the inner cylindrical chamber (65) through the at least one side liquid supply port (I) (80) at a load side pressure ( I) from 8,000 to 20,000 kPa. Most preferably, the iso side liquid component of (I) is introduced into the inner cylindrical chamber (65) through the at least one side liquid supply port (I) (80) at a pressure of side load (I) of 10,000 to 17,000 kPa. Preferably, in the process of the present invention, at least one of the poly (P) side liquid component and the iso (I) side liquid component may optionally contain additional liquid materials. For example, at least one of the poly (P) side liquid component and the iso (I) side liquid component may contain liquid materials selected from the group consisting of foaming agents (e.g., foaming agents). carbamate type such as the Specflex ™ NR 556 CO2 / adduct CO2 / Aliphatic amine adduct available from The Dow Chemical Company); catalysts (e.g., tertiary amine catalysts such as Dabco® 33LV catalyst available from Air Products, Inc., and tin catalyst such as Fomrez tin Momentive catalyst); and surfactants (eg, Evonik's Tegostab® silicone surfactant). Preferably, in the process of the present invention, the poly (P) side liquid component contains an additional liquid material. More preferably, in the process of the present invention, the side poly liquid component (P) contains an additional liquid material; wherein the additional liquid material is at least one of a catalyst and a surfactant. Most preferably, in the process of the present invention, the poly (P) side liquid component contains a catalyst and a surfactant. Preferably, in the process of the present invention, the pressurized gas used is selected from the group consisting of carbon dioxide, nitrogen, air and argon. More preferably, the pressurized gas used is selected from the group consisting of carbon dioxide, nitrogen and air. Even more preferably, the pressurized gas used is selected from the group consisting of nitrogen and air. Most preferably, the pressurized gas used is air.
[0032] Preferably, in the process of the present invention, the pressurized gas used has a water content of 10 ppm. More preferably, the pressurized gas used has a water content of <1 ppm. Even more preferably, the pressurized gas used has a water content of 0.1 ppm. Most preferably, the pressurized gas used has a water content of 0.01 ppm.
[0033] Preferably, in the process of the present invention, the pressurized gas is introduced into the inner cylindrical chamber (65) through the at least two tangential pressurized gas supply ports (85) with an inlet velocity, the An inlet speed of 50 to 600 m / s calculated on the basis of perfect gas conditions at 20 ° C and a pressure of 1 atm, or preferably 75 to 350 m / s. Without wishing to be bound by theory, it should be noted that when the input speed is too low, the polishing layer deposited in the mold 10 has an increased probability of developing undesirable cracks. Preferably, in the process of the present invention, the pressurized gas is introduced into the inner cylindrical chamber (65) through the at least two tangential pressurized gas supply ports (85) with a feed pressure of 150 to 1500 kPa. More preferably, the pressurized gas is introduced into the inner cylindrical chamber (65) through the at least two tangential pressurized gas supply ports (85) with a supply pressure of 350 to 1000 kPa. Most preferably, the pressurized gas is introduced into the inner cylindrical chamber (65) through the at least two tangential pressurized gas supply ports (85) with a supply pressure of 550 to 830 kPa.
[0034] Preferably, the method of forming a chemical mechanical polishing pad polishing layer of the present invention comprises: providing a poly (P) side liquid component and an iso side liquid component (I); wherein the poly-side liquid component (P) and the iso-side liquid component (I) are provided in a stoichiometric ratio of the reactive hydrogen groups (i.e., the total amine groups (NH 2) and groups hydroxyl (OH)) in the components of the poly (P) side liquid component to the unreacted isocyanate groups (NCO) in the iso (I) side liquid component of 0.85 to 1.15 (so more preferably, from 0.90 to 1.10, most preferably from 0.95 to 1.05).
[0035] Preferably, in the process of the present invention, the combined mass flow rate of the poly-side liquid component (P) and the iso-side liquid component (I) in the inner cylindrical chamber (65) is from 1 to 500 g / s (preferably, 25 to 40 g / sec, more preferably 2 to 25 g / sec). Preferably, in the process of the present invention, the ratio of (a) total combined mass flow rate of the poly (P) side liquid component and the iso (I) side liquid component in the inner cylindrical chamber (65) relative to the (b) mass flow rate of the pressurized gas in the inner cylindrical chamber (65) (calculated on the basis of perfect gas conditions at 20 ° C and 1 atm pressure) is <46 to 1 ( more preferably, <30 to 1). Preferably, in the process of the present invention, the combination formed in the axial mixing device (60) is discharged from the open end (68) of the inner cylindrical chamber (65) towards the polishing side (37). ) of the first polishing layer component (32) at a speed of 10 to 300 m / s, filling the plurality of periodic cavities (40) with the combination and allowing the combination to solidify to form a composite structure (58). ). More preferably, the combination is discharged from the opening (69) to the open end (68) of the axial mixing device (60) with a velocity having a component z in a direction parallel to the z axis ( Z) to the polishing side (37) of the first component of the polishing layer (32) from 10 to 300 m / s, filling the plurality of periodic cavities (40) with the combination and allowing the combination of solidifying to form a composite structure (58). (See Figure 9). Preferably, in the process of the present invention, the combination is discharged from the open end (68) of the axial mixing device (60) to an elevation, E, in the z-dimension above the polishing side (37). ) of the first component of the polishing layer (32). More preferably, the combination is discharged from the open end (68) of the axial mixing device (60) on an elevation 3037836 43 E; the average elevation, E, being from 2.5 to 125 cm (more preferably from 7.5 to 75 cm, most preferably from 12.5 to 50 cm). (See Figure 9). Preferably, in the process of the present invention, the combination formed in the axial mixing device has a gel time of 5 to 900 seconds. More preferably, the combination formed in the axial mixing device has a gel time of 10 to 600 seconds. Most preferably, the combination formed in the axial mixing device has a gel time of 15 to 120 seconds. One of ordinary skill in the art will know how to choose a chemical-mechanical polishing pad composite layer (90) having a polishing layer thickness, Tp, suitable for use in a chemical mechanical polishing pad (200). ) for a given polishing operation. Preferably, the chemical-mechanical polishing pad composite polishing layer (90) has an average polishing layer thickness, Tp_avg, along an axis (98) perpendicular to a plane (99) of the polishing surface (95). ). More preferably, the average thickness of the polishing layer, Tp_avg, is 0.51 to 3.81 mm (20 to 150 mils) (more preferably 0.76 to 3.05 mm). at 125 mils), most preferably from 1.00 to 3.05 mm (40 to 120 mils)). Most preferably, the average thickness of the polishing layer, Tp_avg, is equal to the average thickness of the first component, Ti_avg. (See Figures 3 and 10-11). Preferably, the second polishing layer component (45) is a second polymeric non-fugitive phase (50) occupying the plurality of periodic cavities (40) in the chemical-mechanical polishing pad composite polishing layer (90) of the present invention having a height H, measured perpendicular to the polishing surface (95) from the bottom surface (92) of the polishing layer (90) towards the polishing surface (95). Preferably, the second component of the polishing layer (45) is a second non-fugitive polymeric phase (50) occupying the plurality of periodic cavities (40) having a mean height, Hg, measured perpendicular to the polishing (95) from the bottom surface (92) of the polishing layer (90) toward the polishing surface (95); where the absolute value of the difference, AS, between the average thickness of the polishing layer, Tp_avg, and the average height, Havg, is <0.5 μm. More preferably, the absolute value of the difference, AS, is 0.2 μm. Even more preferably, the absolute value of the difference, AS, is 0.1 μm. Most preferably, the absolute value of the difference, AS, is <0.05 μm. (See, for example, Figure 11).
[0036] Preferably, the second component of the polishing layer (45) is a second non-fugitive polymeric phase (50) which occupies the plurality of periodic cavities (40) in the first continuous non-fugitive polymeric phase (30) of the first component of the polishing layer (32), where there are chemical bonds between the first continuous non-fugitive polymeric phase (30) and the second non-fugitive polymeric phase (50). More preferably, the second non-fugitive polymeric phase (50) occupies the plurality of periodic cavities (40) in the first continuous non-fugitive polymeric phase (30), where there are covalent bonds between the first continuous non-fugitive polymeric phase (30) and the second non-fugitive polymeric phase (50) so that the phases can not be separated unless the covalent bonds between the phases are broken.
[0037] Preferably, in the process of the present invention, the combination solidifies as a second component of the polishing layer (45) in the plurality of cavities (40) to form a composite structure (58); wherein the second component of the polishing layer (45) is a second polymeric non-fugitive phase (50); and the chemical-mechanical polishing pad composite polishing layer (90) originates from the composite structure (58), wherein the chemical-mechanical polishing pad composite polishing layer (90) has a polishing surface (95) on the polishing side (37) of the first component of the polishing layer (32); wherein the polishing surface (95) is adapted for polishing a substrate. Preferably, in the method of the present invention, obtaining the chemical-mechanical polishing pad composite polishing layer (90) from the composite structure (58) further comprises: machining the structure composite (58) for obtaining the composite polishing layer of chemical mechanical polishing pad (90). More preferably, machining the composite structure (58) to obtain the chemical-mechanical polishing pad composite polishing layer (90), wherein the chemical-mechanical polishing pad composite polishing layer (90) thus obtained at an average polishing layer thickness, Tp_avg, measured perpendicular to the polishing surface (95) from the bottom surface (92) to the polishing surface (95); where the average thickness of the first component, T1-avg equals the average thickness of the polishing layer, TP-avg; wherein the second non-fugitive polymeric phase occupying the plurality of periodic cavities has a mean height, Havg, measured perpendicularly to the polishing surface (95) from the bottom surface (92) toward the polishing surface (95) ; and wherein an absolute value of a difference, AS, between the average thickness of the polishing layer, Tp-avg, and the average height, Havg, is 0.5 μm (preferably, 0.2 μm; more preferred, <0.1 μm, most preferably 0.05 μm). (See, for example, Figure 11). Preferably, in the method of the present invention, the composite structure (58) is machined by at least one of abrasion (e.g., using a diamond conditioning disc); the cut ; milling (for example, using rotating cutting bits on a milling machine); turning (e.g., with stationary cutting bits applied to a rotating composite structure (58)) and slicing. More preferably, in the method of the present invention, the composite structure (58) is machined by at least one of milling and turning to obtain the composite polishing layer of chemical mechanical polishing pad (90). . Preferably, the chemical-mechanical polishing pad composite polishing layer (90) prepared using the method of the present invention is adapted for polishing a substrate; wherein the substrate is at least one of a magnetic substrate, an optical substrate and a semiconductor substrate. More preferably, the chemical-mechanical polishing pad composite polishing layer (90) prepared using the method of the present invention is adapted for polishing a substrate; wherein the substrate 15 is a semiconductor substrate. Most preferably, the chemical-mechanical polishing pad composite polishing layer (90) prepared using the method of the present invention is adapted for polishing a substrate; the substrate being a semiconductor wafer. Preferably, in the method of the present invention, the chemical-mechanical polishing pad composite polishing layer has a polishing surface having a groove pattern formed in the polishing surface. Preferably, the groove pattern comprises one or more grooves disposed on the polishing surface so that by rotating the composite polishing pad of the chemical mechanical polishing pad during polishing, the one or more grooves sweep the surface. substrate that is polished. Preferably, one or more grooves are curved grooves, linear grooves, and combinations thereof. Preferably, the groove pattern comprises a plurality of grooves. More preferably, the groove pattern is selected from a pattern of grooves. Preferably, the groove pattern is selected from the group consisting of concentric grooves (which may be circular or spiral), curved grooves, cross grooves (e.g., arranged as an XY grid on the surface of the pad ), other regular configurations (e.g., hexagons, triangles), tire tread pattern patterns, irregular patterns (e.g., a fractal pattern), and combinations thereof. More preferably, the configuration in the group consisting of concentric grooves, spiral grooves, grooves is chosen random, grooves of cross grooves, XY grid grooves, hexagonal grooves, triangular grooves, fractal grooves and their combinations. Most preferably, the polishing surface has a spiral groove pattern formed therein. The profile of the groove is preferably selected from a rectangular profile with straight side walls or the cross section of the groove may be V-shaped, U-shaped, sawtooth and combinations thereof. Preferably, the groove pattern comprises a plurality of grooves formed in the polishing surface of a chemical-mechanical polishing pad composite polishing layer, wherein the plurality of grooves are curved grooves. Preferably, the groove pattern comprises a plurality of grooves formed in the polishing surface of a buffer composite polishing layer where the plurality of concentric circular grooves. The groove pattern preferably comprises a plurality of grooves formed in the polishing surface of a chemical-mechanical polishing pad composite polishing layer, wherein the plurality of grooves is consisting of XY linear grooves. Preferably, the groove pattern comprises a plurality of grooves formed in the polishing surface of a chemical-mechanical polishing pad composite polishing layer, wherein the plurality of grooves are concentric circular grooves and XY linear grooves. .
[0038] Preferably, the chemical-mechanical polishing pad composite polishing layer (90) has at least one groove (105) formed in the polishing surface (95) open at the polishing surface (95) and having a groove depth, Gdepth, from the polishing surface (95) measured perpendicular to the polishing surface (95) from the polishing surface (95) towards the bottom surface (92). More preferably, the at least one groove (105) has a mean groove depth of 0.25 mm (10 mils), preferably 0.25 to 3.81 mm (10 to 10 mm). 150 mils)). Even more preferably, the at least one groove (105) has an average groove depth, Gdep th-avg <the average depth of the plurality of periodic cavities, Davg. Preferably, the at least one groove (105) has a mean groove depth, Gdepth-avg> the average depth of the plurality of periodic cavities, Davg. Preferably, the at least one groove (105) forms a groove pattern which comprises at least two grooves (105) having a combination of a groove average depth, Gdep th-avg / 20 selected from 0.25 mm (10). mils), 0.38 mm (15 mils) and 0.38 to 3.81 mm (15 to 150 mils); a width selected from 0.25 mm (10 mils) and 0.25 to 2.5 mm (10 to 100 mils); and a spacing selected from 0.76 mm (30 mils), 41.27 mm (50 mils), 1.27 to 5.10 mm (50 to 200 mils), 1.78 to 5.10 mm (70 to 25 mils), and 200 mils) and 2.29 to 5.10 mm (90 to 200 mils). Preferably, the at least one groove (105) is selected from (a) at least two concentric grooves; (b) at least one spiral groove; (c) a cross groove pattern; and (d) a combination thereof. (See Figures 12, 13a and 13b).
[0039] Preferably, the chemical-mechanical polishing pad composite polishing layer (90) prepared according to the method of the present invention has an average polishing layer thickness, Tp_avg, of 0.51 to 3.81 mm (20 to 20 mm). 150 mils). More preferably, the chemical-mechanical polishing pad composite polishing layer (90) prepared according to the method of the present invention has an average thickness of the polishing layer, Tp_avg, of 0.76 to 3.17 mm. (30 to 125 mils) (even more preferably, from 40 to 120 mils), most preferably from 1.27 to 2.50 mm (50 to 100 mils). mils)). (See Figure 3) Preferably, in the method of the present invention, the provision of the first component of the polishing layer further comprises: providing a mold (10) having a bottom (12) and a peripheral wall (15), the bottom (12) and the peripheral wall (15) defining a mold cavity (20); providing a continuous phase first isocyanate-terminated urethane prepolymer having 8 to 12% by weight of unreacted NCO groups, a continuous first phase curing agent and optionally a plurality of hollow core polymeric material; mixing the isocyanate-terminated urethane prepolymer of the first continuous phase and the first-phase curing agent to form a mixture; pouring the mixture into the mold cavity (20); solidifying the mixture into a cake of the first continuous non-fugitive polymeric phase; obtaining a sheet from the cake (preferably, obtaining a plurality of sheets of the cake); forming the plurality of periodic cavities in the sheet to provide the first component of the polishing layer (preferably, forming the plurality of periodic cavities in the plurality of sheets to provide a plurality of first components of the polishing). More preferably, the plurality of hollow core polymeric materials is incorporated in the first continuous non-fugitive polymeric phase at 1 to 58% by weight. (See Figure 1)
[0040] Preferably, in the method of the present invention, the mold cavity (20) has a central axis, Caris, (22) which coincides with the z axis and intersects the horizontal inner border (14) of the bottom (12). ) of the mold (10) at a central point (21). Preferably, the center point (21) is located at the geometric center of the cross-section, Cx-sectr (24) of the mold cavity (20) projected on the x-y plane (28). (See Figure 1)
[0041] Preferably, the cross-sectional area of the x-y plane-projected cavity (Cx) I (24) may be of any regular or irregular two-dimensional shape. Preferably, the cross-section of the mold cavity Cx_sect (24) is selected from a polygon and an ellipse. More preferably, the cross-section of the mold cavity, Cx-secti (24) is a substantially circular cross section having a mean radius, r, (preferably, where rc is 20 to 100 cm; preferred, wherein rc is 25 to 65 cm, most preferably where rc is 40 to 60 cm). Most preferably, the mold cavity (20) approaches a region having the shape of a straight cylinder having a substantially circular cross section, Cx-sect; wherein the mold cavity has an axis of symmetry, Cx-s, (25) which coincides with the central axis of the mold cavity, Caxis, (22); wherein the straight cylindrical region has a cross-sectional area, Cx-areai defined as follows: Cx-area = nrc2 I 20 where rc is the mean radius of the cross-sectional area of the mold cavity, Cx-areaf projected on the xy plane (28); and wherein re is 20 to 100 cm (more preferably 25 to 65 cm, most preferably 40 to 60 cm). (See Figure 1)
[0042] Preferably, the chemical-mechanical polishing pad composite polishing layer prepared according to the method of the present invention may be made to interface with at least one additional layer to form a chemical mechanical polishing pad. Preferably, the chemical-mechanical polishing pad composite polishing layer prepared according to the method of the present invention is made to interface with a sub-pad (220) using a stacking adhesive (210). Preferably, the sub-pad (220) is made of a material selected from the group consisting of open cell foam, closed cell foam, woven material, nonwoven material (eg, felted, spunbond or needled material), and their 3037836 51 combinations. One of ordinary skill in the art will be able to select a suitable sub-construction material and sub-pad thickness Ts for use as a sub-pad (220). Preferably, the subpad has an average subsamper thickness (220), Ts.sub.sg, of 0.38 (15 mils) (more preferably 0.76 to 2.54 mm (30 to 100 mils). most preferably from 30 to 75 mils (see Fig. 11), those skilled in the ordinary art will know how to choose a stacking adhesive suitable for use in Preferably, the stacking adhesive is a hot melt adhesive, more preferably the stacking adhesive is a hot melt reactive adhesive, more preferably the hot melt adhesive. is a cured reactive hot melt adhesive which has a melt temperature in its uncured state of 50 to 150 ° C, preferably 115 to 135 ° C and has a turnaround time of 90 minutes after melting. all, the reactive hot melt adhesive in its uncured state includes a polyurethane resin (eg, Mor-Melt 'R5003 available from The Dow Chemical Company). Preferably, the chemical-mechanical polishing pad of the present invention is adapted to be made to form an interface with a platen of a polishing machine. Preferably, the chemical-mechanical polishing pad is adapted to be attached to the tray of a polishing machine. More preferably, the chemical mechanical polishing pad may be attached to the tray using at least one of a pressure sensitive adhesive and a vacuum. Preferably, the chemical-mechanical pad (200) comprises a pressure-sensitive tray adhesive (230) applied to the sub-pad (220). One of ordinary skill in the art will know how to choose a pressure sensitive adhesive suitable for use as a pressure sensitive tray adhesive. Preferably, the chemical mechanical polishing pad will also include a release layer (240) applied to the pressure-sensitive tray adhesive (230), the pressure-sensitive tray adhesive (230) being interposed therebetween. between the sub-pad (220) and the separation layer (240). (See Figure 11).
[0043] An important step in substrate polishing operations is the determination of an end point of the process. A conventional in situ method for endpoint detection is to provide a polishing pad with a window that is transparent for selected wavelengths of light.
[0044] During polishing, a light beam is directed through the window at the surface of the wafer where it reflects and passes through the window to a detector (eg, a spectrophotometer). On the basis of the feedback signal, the properties of the surface of the substrate (e.g., the thickness of the films thereon) can be determined for the detection of the end point. To facilitate these light-based endpoint detection methods, the chemical-mechanical polishing pad (200) of the present invention further optionally comprises an end-point detection window (270). Preferably, the end point detection window is chosen from an integrated window incorporated in the composite polishing layer; and an endpoint detection window block placed in place embedded in the chemical mechanical polishing pad. Those of ordinary skill in the art will be able to choose a suitable construction material for the end point detection window for use in the intended polishing process. (See Figure 14) Embodiments of the present invention will now be described in detail in the following examples. Examples 1 to 3: Chemical Mechanical Polishing Pads Commercial polyurethane polishing pads were used as the first continuous non-fugitive phase in the mechano-chemical polishing pads prepared according to each of Examples 1 to 3. Example 1, a commercial IC1000TM polyurethane polishing pad 3037836 53 having a plurality of concentric circular periodic cavities having an average cavity depth, Davg, of 30 mil (0.76 mm), width of 1.52 mm (60 mils) and a spacing of 3.05 mm (120 mils) was provided as the first continuous non-fugitive polymeric phase. In Example 2, a commercial polyurethane polishing pad VP5000TM having a plurality of concentric circular cavities having an average cavity depth, Davg, of 0.76 mm (30 mils), a width of 0.89 mm (35 mils and a spacing of 1.78 mm (70 mils) was provided as the first continuous non-fugitive polymeric phase. In Example 3, a VP5000TM polyurethane polishing pad having a plurality of concentric circular cavities having an average cavity depth, Davg, of 0.76 mm (30 mils), a width of 1.52 mm (60 mils). and a spacing of 3.05 mm (120 mils) was provided as the first continuous non-fugitive polymeric phase. A poly (P) side liquid component was provided, containing: 77.62% by weight of high molecular weight polyether polyol (Voraluxe HF 505 polyol available from The Dow Chemical Company); 21.0% by weight of monoethylene glycol; 1.23% by weight of a silicone surfactant (Tegostab surfactant B8418 available from Evonik) 0.05% by weight of a tin catalyst (Fomrez UL-28 available from Momentive) ; and 0.10% by weight of a tertiary amine catalyst (Dabco 33LV catalyst available from Air Products, Inc.). An additional liquid material (Specflex ™ NR 556 aliphatic amine CO2 / amine adduct available from The Dow Chemical Company) was added to the poly (P) side liquid component at 4 parts per 100 parts by weight of liquid component. poly (P) side. An iso (I) side liquid component was provided, containing: 100% by weight of a modified diphenylmethane diisocyanate (MDI prepolymer IsonateTM 181 available from The Dow Chemical Company.) A pressurized gas (dry air) was provided.
[0045] A second non-fugitive polymeric phase was then provided in the plurality of concentric circular cavities of each of the continuous first non-fugitive polymeric phase materials using an axial mixing device (MicroLine 45 CSM axial mixing device available from US Pat. Hennecke GmbH) having a side liquid supply port (P), a side liquid supply port (I) and four tangential pressurized gas supply ports. The poly-side liquid component (P) and the iso-side liquid component (I) were loaded into the axial mixing device through their respective supply ports with a side charge pressure (P) of 12,500 kPa. a side charge pressure (I) of 17,200 kPa and a weight ratio of (I) / (P) of 1,564 (giving a stoichiometric ratio of NCO reactive hydrogen groups of 0.95). The pressurized gas was charged through the tangential pressurized gas supply ports with a supply pressure of 830 kPa to give a mass flow ratio of the gas-combined liquid components in the axial mixing device of 3.8 1 to form a combination. The combination was then removed from the axial mixing device to each of the first continuous non-fugitive polymeric phases noted at a rate of 254 m / s to fill the plurality of cavities and form composite structures. The composite structures were cured for 16 hours at 100 ° C. The composite structures were then machined on a lathe to give chemical-mechanical polishing pads of Examples 1 to 3. The polishing surfaces of each of the chemical-mechanical polishing pads of Examples 1 to 3 were then grooved for give an XY groove pattern having a groove width of 1.78 mm (70 mils), a groove depth of 0.81 mm (32 mils) and a spacing of 14.73 mm (580 mils).
[0046] Open Porosity 3037836 The open cell porosity of the IC1000TM commercial polishing pad polishing layers and polishing buffers of the VP5000TM polishing pad is reported to be <3% in vol. The porosity of the open cells of the second non-fugitive polymeric phase formed in the mechano-chemical polishing pads in each of Examples 1 to 3 was> 10% in vol. COMPARATIVE EXAMPLES PC1-PC2 AND EXAMPLES P1-P3 Experiments on the speed of removal of chemical mechanical polishing Silicon dioxide polishing removal speed tests were carried out with the chemical mechanical polishing pads prepared according to each of the examples. 1 to 3 and 15 compared with those obtained in Comparative Examples PC1 to PC2 using IC1000TM polyurethane polishing pad and VP5000TM (both commercially available from Rohm and Haas CMP Electronic Materials Inc.) and each having same XY groove pattern noted in the Examples. Specifically, the rate of silicon dioxide removal for each of the polishing pads is shown in TABLE 3. The polishing shrinkage speed experiments were performed on Novellus 200 mm blanket TEOS S15KTEN foil slabs. Systems, Inc.
[0047] A 200 mm Mirra® Applied Materials polishing apparatus was used. All polishing experiments were performed with a pressing force of 8.3 kPa (1.2 psi), a suspension rate of 200 ml / min (ACuPlane ™ 5105 suspension available from Rohm and Haas Electronic Materials CMP 30 Inc. .), a table rotation speed of 93 t / m and a support rotation speed of 87 t / m. A Saesol 8031C diamond pad conditioner (commercially available from Saesol Diamond Ind. Co., Ltd.) was used to condition the polishing pads. The polishing pads were each honed with the conditioner using a 31.1 N pressing force for 10 minutes. The polishing pads were further conditioned at 50% during polishing at 10 scans / min from 1.7 to 9.2 from the center of the polishing pad with a pressing force of 31.1. N. The shrinkage rates were determined by measuring the film thickness before and after polishing using a KLA-Tencor FX200 metrology tool applying a 49-point spiral sweep with a 3 mm edge exclusion. . Each of the withdrawal speed experiments was performed three times. The average withdrawal rate for the triple withdrawal rate experiments for each of the polishing pads is shown in TABLE 3. TABLE 3 Ex # Polishing Buffer TEOS (kmin) Electrochemical PC1 IC1000TM Pad 321 Removal Rate PC2 VP5000TM pad 199 P1 Ex. 1 (1521A) 426 P2 Ex. 2 (1521B) 355 P3 Ex. 3 (1521C) 304 15

权利要求:
Claims (10)
[0001]
REVENDICATIONS1. A method of forming a composite polishing layer of a chemical mechanical polishing pad, comprising: providing a first polishing layer component of the composite polishing layer of a chemical mechanical polishing pad; wherein the first polishing layer component has a polishing side, a base surface, a plurality of periodic cavities and an average thickness of the first component, T1_ measured perpendicularly with respect to the polishing side from the base surface to the polishing side; Wherein the first polishing layer component comprises a first continuous non-fugitive polymeric phase; wherein the plurality of periodic cavities have an average cavity depth, D aVg, measured perpendicularly to the polishing side from the polishing side towards the base surface, where the average cavity depth, Dag, is less than the average thickness of the first component, Ti-avg; wherein the first continuous non-continuous polymeric phase is a reaction product of a continuous first phase isocyanate-terminated urethane prepolymer having 8 to 12% by weight of unreacted NCO groups and a curing agent. first continuous phase; providing a poly (P) side liquid component comprising at least one of a side polyol (P), a side polyamine (P) and an amine side alcohol (P); providing an iso (I) side liquid component comprising at least one polyfunctional isocyanate; the supply of a pressurized gas; providing an axial mixing device having an internal cylindrical chamber; wherein the inner cylindrical chamber has a closed end, an open end, an axis of symmetry, at least one side liquid supply port (P) which opens into the inner cylindrical chamber, at least one a side liquid supply (I) which opens into the internal cylindrical chamber, and at least one tangential pressurized gas supply port which opens into the inner cylindrical chamber where the closed end and the open end are perpendicular to the axis of symmetry where the at least one side chamber side liquid supply port (P) is closed; wherein and the at least one liquid supply port (I) is disposed along a circumference of the inner cylindrical near the end the at least one tangential pressurized gas supply port is disposed along a circumference of the chamber cylindrical internal downstream of the at least one side liquid supply port (P) and the at least one side liquid supply port (I) from the closed end; wherein the poly-side liquid component (P) is introduced into the inner cylindrical chamber through the at least one side liquid supply port (P) at a side charge pressure (P) of 6,895 to 27,600 kPa ; wherein the iso-side liquid component (I) is introduced into the inner cylindrical chamber through the at least one side liquid supply port (I) at a side load pressure (I) of 6,895 to 27,600 kPa; wherein a combined mass flow rate of the poly-side liquid component (P) and the iso-side liquid component (I) in the inner cylindrical chamber is from 1 to 500 g / s; wherein the poly-side liquid component (P), the iso-side liquid component (I) and the pressurized gas are mixed in the inner cylindrical chamber to form a combination where the pressurized gas is introduced into the inner cylindrical chamber through the minus a tangential pressurized gas supply port with a supply pressure of 150 to 1500 kPa; wherein an inlet velocity in the internal cylindrical chamber of pressurized gas is 50 to 600 m / s calculated on the basis of perfect gas conditions at 20 ° C and a pressure of 1 atm; evacuating the combination of the open end of the inner cylindrical chamber towards the polishing side of the first polishing layer component at a speed of 5 to 1000 m / s, filling the plurality of periodic cavities with combining, solidifying the combination as a second polishing layer component in the plurality of periodic cavities to form a composite structure; wherein the second polishing layer component is a second non-fugitive polymeric phase; and, obtaining a chemical-mechanical polishing pad composite polishing layer from the composite structure, wherein the chemical-mechanical polishing pad composite polishing layer has a polishing surface on the polishing side of the first polishing layer component and wherein the polishing surface is adapted for polishing a substrate.
[0002]
The method of claim 1, further comprising: machining the composite structure to obtain the composite polishing layer of a chemical mechanical polishing pad; wherein the composite polishing layer of a chemical-mechanical polishing pad thus obtained has an average thickness of composite polishing layer, Tp_avg, measured perpendicular to the polishing surface from the base surface to the polishing surface ; where the average thickness of the first component, T-1-avg equals the average thickness of the composite polishing layer, Tp_ avg; Wherein the second non-fugitive polymeric phase occupying the plurality of periodic cavities has an average height, Hg, measured perpendicularly to the polishing surface from the base surface toward the polishing surface; and, where an absolute value of a difference, AS, between the average thickness of the composite polishing layer, Tp_avg, and the average height, Havg, is 0.5 μm. 10
[0003]
The method of claim 2, further comprising: forming at least one groove in the polishing surface. 15
[0004]
The method of claim 1, wherein providing the first polishing layer component further comprises: providing a mold having a bottom and a peripheral wall, wherein the bottom and the peripheral wall defining a mold cavity; Providing a continuous phase first isocyanate-terminated urethane prepolymer having 8 to 12% by weight of unreacted NCO groups, continuous first phase curing agent and optionally, a plurality of hollow core polymeric materials; Mixing the continuous phase first isocyanate-terminated urethane prepolymer and the first continuous phase curing agent to form a mixture; pouring the mixture into the mold cavity; Solidifying the mixture into a cake of the first continuous non-fugitive polymeric phase; obtaining a sheet from the cake; forming the plurality of periodic cavities in the sheet to provide the first polishing layer component. 3037836 61
[0005]
The method of claim 4, wherein the plurality of hollow core polymeric materials is incorporated in the first non-fugitive polymeric phase continues at 1 to 58% by vol. 5
[0006]
The method of claim 1, wherein the poly (P) side liquid component comprises 25 to 95% by weight of a side polyol (P); wherein the side polyol (P) is a high molecular weight polyether polyol; wherein the high molecular weight polyether polyol has a number average molecular weight, MN, of 2,500 to 100,000 and an average of 4 to 8 hydroxyl groups per molecule.
[0007]
The process of claim 1 wherein the iso (I) side liquid component comprises a polyfunctional isocyanate having an average of two reactive isocyanate groups per molecule.
[0008]
The process of claim 1 wherein the pressurized gas is selected from the group consisting of CO2, N2, air and argon.
[0009]
The method of claim 1, wherein the inner cylindrical chamber has a circular cross section in a plane perpendicular to the axis of symmetry of the inner cylindrical chamber; wherein the open end of the inner cylindrical chamber has a circular opening perpendicular to the axis of symmetry of the inner cylindrical chamber; where the circular aperture is concentric with the circular cross section; and wherein the circular aperture has an internal diameter of 2.5 to 6 mm.
[0010]
The method of claim 1, wherein the polishing surface is adapted to polish a semiconductor wafer.

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同族专利:

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公开号 | 公开日

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CN107695869A|2018-02-16|

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DE102016007772A1|2016-12-29|

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US20160375554A1|2016-12-29|

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TWI719028B|2021-02-21|

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CN107695869B|2019-06-21|

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TW201700556A|2017-01-01|

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JP2017052079A|2017-03-16|

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US10092998B2|2018-10-09|

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KR20170001627A|2017-01-04|

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JP6783562B2|2020-11-11|

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法律状态:
2017-05-11| PLFP| Fee payment|Year of fee payment: 2 |

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2018-05-11| PLFP| Fee payment|Year of fee payment: 3 |

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2019-05-10| PLFP| Fee payment|Year of fee payment: 4 |

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2020-07-17| RX| Complete rejection|Effective date: 20200610 |

优先权:

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申请号 | 申请日 | 专利标题

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US14/751,410|US10011002B2|2015-06-26|2015-06-26|Method of making composite polishing layer for chemical mechanical polishing pad|

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US15/163,184|US10092998B2|2015-06-26|2016-05-24|Method of making composite polishing layer for chemical mechanical polishing pad|

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