CN114029856A - Chemical mechanical polishing pad with high end point detection precision, preparation method and application thereof - Google Patents

Chemical mechanical polishing pad with high end point detection precision, preparation method and application thereof Download PDF

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Publication number
CN114029856A
CN114029856A CN202111437207.1A CN202111437207A CN114029856A CN 114029856 A CN114029856 A CN 114029856A CN 202111437207 A CN202111437207 A CN 202111437207A CN 114029856 A CN114029856 A CN 114029856A
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layer
polishing pad
polishing
detection window
window
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CN114029856B (en
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谢毓
王凯
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Wanhua Chemical Group Electronic Materials Co ltd
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Wanhua Chemical Group Electronic Materials Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/11—Lapping tools
    • B24B37/20—Lapping pads for working plane surfaces
    • B24B37/22—Lapping pads for working plane surfaces characterised by a multi-layered structure
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/11—Lapping tools
    • B24B37/20—Lapping pads for working plane surfaces
    • B24B37/24—Lapping pads for working plane surfaces characterised by the composition or properties of the pad materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • B24B37/11—Lapping tools
    • B24B37/20—Lapping pads for working plane surfaces
    • B24B37/26—Lapping pads for working plane surfaces characterised by the shape of the lapping pad surface, e.g. grooved
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
    • B24D18/009—Tools not otherwise provided for
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
    • B29C39/02—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor for making articles of definite length, i.e. discrete articles
    • B29C39/10—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor for making articles of definite length, i.e. discrete articles incorporating preformed parts or layers, e.g. casting around inserts or for coating articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
    • B29C39/02—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor for making articles of definite length, i.e. discrete articles
    • B29C39/12—Making multilayered or multicoloured articles
    • B29C39/123—Making multilayered articles

Abstract

The invention discloses a chemical mechanical polishing pad with high end point detection precision, a preparation method and application thereof. The chemical mechanical polishing pad has the advantages of high end point detection precision, few polishing defects and the like, and is suitable for chemical mechanical polishing of magnetic substrates, optical substrates or semiconductor substrates.

Description

Chemical mechanical polishing pad with high end point detection precision, preparation method and application thereof
Technical Field
The invention belongs to the technical field of chemical mechanical polishing, and particularly relates to a chemical mechanical polishing pad with high end point detection precision and low surface scratch, a preparation method and application thereof.
Background
In the manufacturing process of integrated circuits and other electronic devices, the method for removing fine irregularities from the surface of a semiconductor wafer is mainly Chemical Mechanical Polishing (CMP). During polishing, a polishing medium is provided between the wafer and the polishing pad, so that the wafer surface is polished and made flat by the chemical and mechanical action of the pad surface and the polishing medium.
In general, an endpoint detection device is used in a CMP process to determine whether a polishing endpoint is reached. In situ endpoint detection is currently more common. In situ optical endpoint detection techniques can be divided into two basic categories: (1) monitoring reflected optical signals at a single wavelength or (2) monitoring reflected optical signals at multiple wavelengths. Conventional wavelengths for optical endpoints include wavelengths within the following ranges: a visible spectrum (e.g., 400-700 nm), an ultraviolet spectrum (315-400 nm), and an infrared spectrum (700-1000 nm).
Patent CN105922126B provides a method for preparing a detection window, which is synthesized from a compound containing bifunctional thiol, resulting in a window with improved light transmittance. The window obtained by the method cannot ensure that the grinding surface facing the surface of the wafer and the grinding surface of the polishing layer have the same grinding physical property, and is easy to generate undesirable scratches in the polishing process.
Patent TW200716303 provides a polishing pad with a window with reduced surface roughness. The surface roughness of the lower surface of the window is reduced by laser ablation treatment, and the light scattering property is reduced, so that the purpose of improving the light transmittance is achieved. The precision and difficulty required in the laser ablation process are high, and the implementation is difficult, and the production efficiency of the product is affected.
Patent CN100347826C discloses a polishing pad with a high light transmission window formed by the reaction of an aliphatic isocyanate, a hydroxyl-containing material and a curing agent, as shown in fig. 1, comprising an upper layer, a lower layer and an intermediate pressure sensitive adhesive layer, wherein the thickness of the window is only the same as the thickness of the upper layer. Due to the hollow structure at the bottom of the window, the deformation of the window due to the recess or protrusion during the polishing process can affect the surface quality of the ground wafer.
Currently, how to accurately judge the polishing endpoint in the polishing process is a very important task. Therefore, the polishing pad with high end point detection precision and small surface scratch generated by the window is still needed urgently.
Disclosure of Invention
To overcome the deficiencies of the prior art, it is an object of the present invention to provide a chemical mechanical polishing pad with a unique endpoint detection window structure that has higher endpoint detection accuracy and lower scratching defects when used in a polishing process.
It is another object of the present invention to provide a method for preparing such a high endpoint detection accuracy, low scratch chemical mechanical polishing pad.
It is a further object of this invention to provide such a high endpoint detection accuracy, low scratch CMP pad application.
In order to achieve the purpose, the invention adopts the following technical scheme:
a chemical mechanical polishing pad with high end point detection precision comprises a polishing layer and a detection window, wherein the detection window is of a sandwich-like structure with a top layer, a middle layer and a bottom layer facing a polishing surface, and the thickness of the detection window is the same as that of the polishing pad; the top layer and the bottom layer are made of the same material and both are made of a polymer matrix material, and the middle layer is made of a high-refractive-index material containing a thiol compound.
In a specific embodiment, the thiol compound contained in the high refractive index material of the intermediate layer is a thiol compound having at least three mercapto groups; preferably, the refractive index of the whole detection window ranges from 1.55 to 1.67.
In a specific embodiment, the polishing layer is comprised of a polymeric matrix material and polymeric microelements; preferably, the polymer matrix material is a thermosetting material, more preferably a polyurethane material, and the polymeric microelements are microspheres; further preferably, the addition amount of the microspheres accounts for 2-5 wt% of the total mass of the polyurethane.
In a specific embodiment, the surface of the polishing layer is provided with a macro structure groove, and the depth of the groove is 0.5-0.8 mm; preferably, the thickness of the top layer of the detection window is greater than or equal to 1/2 of the groove depth of the polishing layer and less than or equal to the groove depth; more preferably, the thickness of the bottom layer of the detection window is greater than 0mm and less than 0.5 mm.
In a specific embodiment, the detection window has a surface shore D hardness within a range of ± 5D of the polishing layer surface shore D hardness; preferably, the compression ratio of the detection window is within ± 0.5% of the compression ratio of the polishing layer.
In a specific embodiment, the polishing pad further comprises an adhesive layer and a buffer layer, wherein the polishing layer and the buffer layer are connected and attached through the adhesive layer, the adhesive layer is selected from one or a combination of a pressure-sensitive adhesive or a hot melt adhesive, and the buffer layer is selected from a polyurethane felt type or a foam type structure layer.
In another aspect, a method for preparing the chemical mechanical polishing pad includes the following steps:
1) from NCO group-containing prepolymers and NH-containing prepolymers2Or OH, and pouring a top layer structure of the detection window, wherein the gel time of the top layer structure is t1，t15-15 min; preferably, wherein NCO is reacted with unreacted NH2Or the molar ratio of OH is 1-1.2;
2) by reaction of isocyanates with thiol compounds at t1-4～t1-casting an intermediate layer structure of the detection window within 2min, the intermediate layer structure having a gel time t2，t25-13 min; preferably, the molar ratio of NCO in isocyanate to SH in thiol compound is 0.9-1.1;
3) from NCO group-containing prepolymers and NH-containing prepolymers2Or OH, at t2-4～t2-casting the substructure within 2 min; preferably, wherein NCO is reacted with unreacted NH2Or the molar ratio of OH is 1-1.2;
preferably, the detection window is prepared by sequentially pouring and molding from step 1) to step 3) from bottom to top or from top to bottom.
In a preferred embodiment, the method further comprises a step of preparing a polishing layer from a prepolymer containing NCO groups and a prepolymer containing NH groups2Or OH curing agent and microsphere curingReacting to obtain; preferably, unreacted NH in the polishing layer2Or the molar ratio of OH to NCO is 0.8-1; more preferably, in the polishing layer, the addition amount of the microspheres is 2-5 wt% of the total mass of the polyurethane.
In a specific embodiment, the detection window is prepared in the same mold, and then the polishing layer is prepared to form a polishing pad with an integral detection window; or preparing the detection window and the polishing layer respectively, then opening a hole on the polishing layer and inserting the detection window to obtain the polishing pad with the insertion-type detection window.
In yet another aspect, the chemical mechanical polishing pad of the foregoing or the foregoing method is used for chemical mechanical polishing of a magnetic, optical or semiconductor substrate.
Compared with the prior art, the chemical mechanical polishing pad has the following beneficial effects:
the window structure of the chemical mechanical polishing pad has a sandwich-like structure, and comprises a top layer structure which is made of the same material as a polishing layer matrix and faces a polishing surface, the top layer structure ensures that the surface, in contact with a wafer, of a detection window has the same grinding property of the contact surface of the polishing layer and the wafer, and the surface of the wafer cannot be scratched due to the change of the polishing performance caused by the change of the material of the detection window; the mercapto compound with the functionality higher than that of the middle layer with high refractive index is added to ensure that a reticular structure is formed among molecules, so that the structural stability of the middle layer is improved, incident detection light waves are reflected less, more refraction enters a detection window and is received by a receiver for end point detection, and the accuracy of optical detection is improved. Because the middle layer is made of different materials, the physical properties of the detection window material can be influenced, so that the bottom layer is filled by the bottom layer material which is made of the same material as the top layer material, and the polishing physical properties of the whole detection window are ensured to be the same as those of the polishing pad.
According to the preparation method of the chemical mechanical polishing pad, in the window pouring process, the top layer structure of the window is poured firstly, the intermediate layer material is poured continuously when the top layer structure is not completely gelled, so that when the top layer polymer is not completely solidified, part of groups react with molecules in the intermediate layer material to generate chemical bonding, and chemical bonding rather than physical bonding is formed at the interface of the two layers, so that on one hand, the connection between the two layers is firmer, the phenomenon that a window block body falls off or separates in the polishing process is avoided, on the other hand, the chemical bonding between the two layers is more beneficial to detecting light penetrating between the two layers, and ineffective dissipation of the light caused by the physical interface is reduced. Similarly, when the middle layer is not completely gelled, the bottom layer material is continuously poured to play the same role. The end point detection window obtained by the process has high light transmission efficiency, firm connection among layers and no need of other binders.
The thickness of the detection window in the chemical mechanical polishing pad is the same as that of the polishing pad, while the thickness of the detection window is the same as that of the polishing layer in the traditional polishing pad with the detection window, so that the window is in a hollow state at the lower part of the polishing pad. The window structure is in a hollow state below the window structure, so that bending deformation is easy to occur in the polishing process, a large amount of polishing liquid is instantly gathered between the wafer and the detection window, the polishing speed is higher than that of the contact part of the wafer and the polishing layer, and the local over-polishing phenomenon is generated, so that the uniformity of the wafer is damaged. The thickness of the sandwich-like shape of the invention is the same as the whole thickness of the polishing pad, thus reducing the problem of the dent generated by the detection window in the polishing process, being beneficial to reducing the defects of scratch and the like of the surface of the wafer and improving the polishing uniformity of the surface of the wafer.
Drawings
FIG. 1 is a schematic side view of a conventional polishing pad.
FIG. 2 is a schematic side view of the polishing pad of the present invention.
Wherein, 1 is a chemical mechanical polishing pad, 2 is a polishing layer, 3 is an adhesive layer, 4 is a buffer layer, 5 is a detection window, 6 is a top layer, 7 is a middle layer, and 8 is a bottom layer.
Detailed Description
The following examples will further illustrate the method provided by the present invention in order to better understand the technical solution of the present invention, but the present invention is not limited to the listed examples, and should also include any other known modifications within the scope of the claims of the present invention.
As shown in fig. 2, a chemical mechanical polishing pad 1 with high end point detection precision comprises a polishing layer 2, an adhesive layer 3, a buffer layer 4 and a detection window 5, wherein the polishing layer 2 and the buffer layer 4 are bonded and pressed through the adhesive layer 3; wherein the detection window 5 has a sandwich-like structure of a top layer 6, a middle layer 7 and a bottom layer 8 facing the polishing surface, and the thickness of the detection window 5 is the same as that of the polishing pad 1; the top layer 6 and the bottom layer 8 of the detection window are made of the same material and both are made of a polymer matrix material, and the middle layer 7 is made of a high-refractive-index material including thiol compounds.
Correspondingly, the polishing layer 2 is composed of a polymer matrix material and a polymer micro-component, wherein the polymer matrix material may be a material commonly used in the art without any limitation, for example, the polymer matrix material is selected from at least one of a segmented block copolymer or a polyurethane elastomer, and is preferably a polyurethane elastomer material. The polymeric microelements are preferably polymeric hollow microspheres, and may be selected from the series of expandable microspheres available from Acksonobel. Specifically, the amount of the hollow polymer microspheres added is 2 to 5 wt%, such as 2 wt%, 2.5 wt%, 3 wt%, 3.2 wt%, 3.4 wt%, 3.6 wt%, 3.8 wt%, 4 wt%, 4.5 wt%, 5 wt%, based on the total weight of the polyurethane of the polishing layer, but not limited thereto, and is preferably 3 to 4 wt%.
The polyurethane elastomer material is obtained by reacting a prepolymer containing unreacted isocyanate groups with a curing agent containing unreacted active hydrogen groups. The prepolymer component containing unreacted isocyanate groups is obtained by reacting a polyisocyanate, such as methylene diphenyl diisocyanate, toluene diisocyanate, naphthalene diisocyanate, p-phenylene diisocyanate, o-toluidine diisocyanate, carbodiimide-modified diphenylmethane diisocyanate, biuret-modified diphenylmethane diisocyanate, isophorone diisocyanate, 1, 6-hexamethylene diisocyanate, 4' -dicyclohexylmethane diisocyanate, cyclohexane diisocyanate, and mixtures thereof, with a polyol, but is not limited thereto. The polyol is, for example, at least any one selected from polytetramethylene ether glycol, polypropylene ether glycol, polycarbonate polyol, polycaprolactone polyol, ethylene adipate or ester-based polyol of butylene adipate, and may also be, for example, a copolymer or a mixture thereof, but is not limited thereto. The curing agent containing active hydrogen groups is a polyol or polyamine curing agent. For example, at least one selected from the group consisting of ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, 1, 2-butylene glycol, 1, 3-butylene glycol, 2-methyl-1, 3-propylene glycol, 1, 4-butylene glycol, 1, 6-hexanediol, diethylene glycol, dipropylene glycol, tripropylene glycol, 4 '-methylene-bis-o-chloroaniline, propylene glycol di-p-aminobenzoate, 2-bis (2-aminophenylthio) ethane, 4' -methylene-bis-aniline, 5-tert-butyl-2, 4-toluenediamine, and 3-tert-butyl-2, 6-toluenediamine, but is not limited thereto.
The curing agent containing unreacted active hydrogen groups may also be selected from diethyltoluenediamine, 3, 5-dimethylthio-2, 4-toluenediamine, 3, 5-diethyltoluenediamine-2, 4-diamine, 3, 5-diethyltoluenediamine-2, 6-diamine, 4' -bis- (sec-butylamino) -diphenylmethane, 1, 4-bis- (sec-butylamino) -benzene; 4,4 ' -methylene-bis- (2-chloroaniline), 4 ' -methylene-bis- (3-chloro-2, 6-diethylaniline), polycyclobutane oxide-di-p-aminobenzoate, N ' -dialkyldiaminodiphenylmethane, p ' -methylenedianiline, m-phenylenediamine, 4 ' -methylene-bis- (2-chloroaniline), 4 ' -methylene-bis- (2, 6-diethylaniline), 4 ' -methylene-bis- (2, 3-dichloroaniline), 4 ' -diamino-3, 3 ' -diethyl-5, 5 ' -dimethyldiphenylmethane, 4 ' -diamino-3, 3 ' -diethyl-5, 5 ' -dimethyldiphenylmethane, and mixtures thereof, Propylene glycol di-p-aminobenzoate, but is not limited thereto.
The polyurethane material of the polishing layer matrix is obtained by reacting a prepolymer containing an NCO group with a curing agent containing an active hydrogen group. In the polishing layer, unreacted NH2Or the molar ratio of OH to NCO is 0.8-1, preferably 0.85-0.95, such as 0.85, 0.9, 0.95, but not limited thereto.
Materials selected for the top and bottom layers of the window andthe polymer matrix materials of the polishing layer are the same and are obtained by reacting a prepolymer containing NCO groups with an active hydrogen group curing agent. Wherein NCO is reacted with unreacted NH2Or the molar ratio of OH is 1 to 1.2, preferably 1.05 to 1.15, such as 1.05, 1.1, 1.15, but not limited thereto. The window interlayer material is obtained by reacting isocyanate and a thiol compound, wherein the molar ratio of NCO in the isocyanate to SH in the thiol compound is 0.9-1.1, preferably 0.95-1.05, such as 0.95, 1, 1.05, but not limited thereto.
The material of the bottom layer of the detection window and the material of the top layer are the same, and the types of the material of the bottom layer of the detection window and the material of the top layer of the detection window are basically the same as the type selection of the base material of the polishing layer, so that the consistency of the grinding performance of the surface of the detection window and the polishing layer is ensured.
The thiol compound contained in the high refractive index material of the window intermediate layer is selected from thiol compounds having at least three mercapto groups; preferred are trimethylolpropane tris (3-mercaptopropionate), trimethylolethane tris (3-mercaptopropionate), pentaerythritol tetrakis (3-mercaptopropionate), and pentaerythritol tetramercaptoacetate, but not limited thereto.
The middle-layer high-refractive-index material is obtained by reacting a thiol compound with at least three mercapto groups with an isocyanate compound, and the molar ratio of unreacted NCO to SH is 0.9-1.1. Such as, but not limited to, 0.9, 1, 1.1.
In the invention, the thickness of the detection window top layer is greater than or equal to 1/2 of the depth of the groove of the polishing layer and less than or equal to the depth of the groove. The surface of the polishing layer has a macro groove structure, and the depth of the groove is 0.5-0.8 mm, preferably 0.55-0.75 mm, such as 0.55mm, 0.6mm, 0.65mm, 0.7mm, 0.75mm, but not limited thereto.
Wherein the surface of the polishing layer has a macro-groove shape, such as a pattern of grooves selected from the group consisting of curvilinear grooves, linear grooves, perforations, and combinations thereof. Preferably, the pattern of grooves comprises a plurality of grooves, such as one selected from the group consisting of: concentric grooves, spiral grooves, cross shadow groove, X-Y grid grooves, hexagonal grooves, triangular grooves, fractal grooves and combinations thereof.
In the invention, the detection window intermediate layer is mainly composed of polythiourethane material obtained by the reaction of polythiol and isocyanate, and the refractive index of the intermediate layer can be adjusted by adjusting the content of sulfur in the material by adjusting the using amount of the polythiol. The middle layer of the detection window is a high refractive index layer, so that the overall refractive index of the upper, middle and lower layers of the detection window is in the range of 1.55-1.67, preferably 1.57-1.63, such as 1.57, 1.60, 1.63, but not limited thereto.
In the present invention, the thickness of the bottom layer of the detection window is greater than 0mm and less than 0.5mm, preferably 0.05-0.3 mm, such as 0.05mm, 0.1mm, 0.15mm, 0.2mm, 0.25mm, 0.3mm, but not limited thereto.
In the present invention, the Shore D hardness of the detection window surface is different from the Shore D hardness of the polishing pad surface by + -5D, preferably + -3D, such as + -1D, + -2D, + -3D, but not limited thereto. The compressibility of the detection window differs from the compressibility of the polishing pad by ± 0.5%, preferably by ± 0.3%, for example, ± 0.1%, ± 0.2%, ± 0.3%, but is not limited thereto.
In the present invention, the cushioning layer may be selected from the group consisting of foam materials, woven materials, and nonwoven materials, including but not limited to felt materials, and needle punched materials, and the like, and may be selected from the SUBA series of materials, for example. The adhesive layer is selected from one or a combination of a hot melt adhesive or a pressure sensitive adhesive. The hot melt adhesive is selected from at least one of polyolefin, ethylene vinyl acetate, polyamide, polyester, polyurethane, polyvinyl chloride or epoxy resin; the pressure-sensitive adhesive is selected from at least one of a propylene-based adhesive (PSAV) or a rubber-based adhesive (PSA 8). The process of bonding and attaching the polishing layer to the buffer layer via the adhesive layer is not particularly limited, and reference may be made to the prior art, which is well known to those skilled in the art.
The preparation method of the window for the chemical mechanical polishing pad with the sandwich-like structure comprises the following steps:
firstly, pouring a top layer structure of a window in a mould, wherein the top layer material has a gel time t1，t1The value range is 5-15 min, preferably 8-13 min, such as 8min, 9min, 10min, 11min, 12min, 13min, but is not limited thereto; then, at t1-4min～t1Pouring the intermediate layer structure material within-2 min, preferably t1-3min～t1-1min, but not limited thereto. The intermediate layer structure has a gel time t2，t2The value range is 5-13 min, preferably 7-10 min, such as 7min, 8min, 9min, 10min, but not limited thereto; finally, at t2-4min～t2Casting the substructure material within-2 min, preferably t2-3min～t2-1min, but not limited thereto. And finally, heating the die to 80-120 ℃ for curing for 6-12 hours, cooling and demolding, and cutting the detection window block into the required size by adopting any cutting mode known by the technical personnel in the field.
The detection window may be an insertion window, or may be an integral window disposed in the polishing pad, and may be disposed in the polishing pad in any manner known to those skilled in the art. The preparation method of the monolithic window polishing pad comprises the steps of firstly preparing the detection window by adopting the preparation method of the window, then curing the detection window in the same mold to obtain the polishing layer, and in the preparation process, a prepolymer, a curing agent and the like of the polishing layer are in contact with and cross-linked with the cured detection window to generate a polymerization reaction and cure, so that the chemical connection of the polishing layer and the detection window is realized, and the polishing pad with the monolithic window structure is formed.
The chemical mechanical polishing pad of the present invention can be applied in chemical mechanical planarization, preferably, but not limited to, chemical mechanical polishing of copper wafers, sapphire wafers, silicon wafers, and wafers.
The invention is further illustrated, but not limited, by the following more specific examples.
Not specifically described, the polishing layers of the examples and comparative examples of the present invention were prepared as follows:
polishing layer: 2876g of prepolymer (PET 95A, Coim company) and 1230g of curing agent 1230g of MOCA (Shanghai Kaiyin) are stirred and mixed uniformly, 125g of 40D60 microspheres produced by Aksu Nobel company are added into the mixture, the mixture is injected into a mold after being stirred rapidly, the mixture is heated to 110 ℃ and cured for 9 hours, and then the mixture is cooled to room temperature and demolded, and the polishing layer sheet is obtained after cutting. And (3) grooving the obtained polishing pad by using a grooving machine to form a macro micro groove on the surface.
Buffer layer: selected from SUBA IV (DOW).
Bonding layer: VHB series tape from 3M company.
And attaching the obtained polishing layer, the bonding layer, the buffer layer and the bonding layer in sequence to obtain the polishing pad without the detection window. The resulting polishing pad is die-cut at an appropriate position to obtain a through-hole in which the inspection window can be placed. The detection window was bonded into the through-hole of the polishing pad by Primer94 glue (3M) to obtain a chemical mechanical polishing pad with an end-point detection window.
The main polishing methods and measuring equipment used in the examples and comparative examples of the present invention were as follows:
equipment: mirraTMCMP polisher.
The polishing method comprises the following steps: a Cu target was polished for one minute by offline conditioning using SS12 polishing solution (manufactured by Kabert Co.) under a head pressure of 1.5psi (10.3kPa) for one minute. The rotation speed of the grinding platform is 70rpm, and the polishing head speed is 60rpm in the polishing process.
And (3) gel time measurement: the test was carried out according to ASTM D3056-85.
Surface scratching: the scratch on the target material in the experimental process is represented by the number of scratch strips with the surface length of the target material being more than 0.5 cm.
Hardness: performing Shore hardness test according to the GB/T531-2008 method.
Compression ratio: compression ratio testing was performed according to ASTM D1229-2003(2008) method.
Light transmittance: the light transmittance of the detection window with the sandwich structure before and after polishing under the D light wavelength is tested according to the GB/T2410-2008 method.
Example 1
The preparation method of the window comprises the following steps: the top layer and the bottom layer of the window are selected from 325g of prepolymer (PET 95A manufactured by Coim company) and 110g of MOCA (Shanghai Kaiyin), and are stirred and mixed uniformly; the interlayer material was chosen from 286g of TDI-100 (Wawa) and 420g of pentaerythritol tetrakis (3-mercaptopropionate) (Jingbo). The gel time of the top/bottom layer material was tested to be 8min and the gel time of the middle layer 8 min. Uniformly mixing the top layer material, pouring into a mold, starting timing, continuously pouring the middle layer material after 6min, pouring the bottom layer material after 6min, putting the poured window into a mold, heating and curing at 100 ℃ for 8h, cooling and demolding to obtain a window block, and cutting the obtained window block into a proper size to be installed in a polishing pad.
The preparation method of the polishing pad comprises the following steps: 2876g of prepolymer (PET 95A of Coim company) and 90g of microspheres (Nobel chemical 40D25) are uniformly stirred and mixed, 1230g of curing agent MOCA (Shanghai Keyin) is added and uniformly stirred, the mixture is injected into a mold and heated to 100 ℃ for 8 hours, and the polishing layer is obtained after slicing. The polishing layer sheet was sequentially attached to a SUBA IV buffer layer (DOW) via PSA3000(3M) to obtain a polishing pad. A window sized hole was punched in the pad using a die and the window block was affixed in the pad hole by hot melt AM158 (Howtec).
The chemical mechanical polishing pad with the detection window is prepared by the method, and concentric circular grooves are engraved on the surface of the polishing pad, wherein the depth of each groove is 0.8mm, and the thickness of the polishing pad is 2.3 mm. The thickness of the top layer of the detection window is 0.45mm, the thickness of the middle layer is 1.65mm, and the thickness of the bottom layer is 0.2 mm. The obtained chemical mechanical polishing pad was subjected to polishing test and various physical property tests.
Example 2
The preparation method of the window comprises the following steps: the top layer and the bottom layer of the window are selected from 287g of prepolymer (PET 95A of Coim company) and 107g of MOCA (Shanghai Kaiyin) and are stirred and mixed evenly; the interlayer material was selected from 195g isophorone diisocyanate (Wawa) and 214g trimethylolpropane tris (3-mercaptopropionate) (Suzhou Navigator). The gel time of the top/bottom layer material was tested to be 8min and the gel time of the middle layer was tested to be 9 min. Uniformly mixing the top layer material, pouring into a mold, starting timing, beginning to continue pouring the middle layer material after 5min, pouring the bottom layer material after 6min, putting the poured window into a 100 ℃ temperature, heating and curing for 8h, cooling and demolding to obtain a window block, and cutting the obtained window block into a proper size to be installed in a polishing pad.
The preparation method of the polishing pad comprises the following steps: 2876g of prepolymer (PET 95A manufactured by Coim company) and 125g of microspheres (Nobel chemical 40D25) are taken and stirred uniformly, then 1315g of curing agent MOCA (Shanghai Keyin) is added and stirred uniformly, the mixture is injected into a mold and heated to 100 ℃ for 8 hours, and a polishing layer is obtained after slicing. The polishing layer sheet was sequentially attached to a SUBA IV buffer layer (DOW) via PSA3000(3M) to obtain a polishing pad. A window sized hole was punched in the pad using a die and the window block was affixed in the pad hole by hot melt AM158 (Howtec).
The chemical mechanical polishing pad with the detection window is prepared by the method, and concentric circular grooves are engraved on the surface of the polishing pad, wherein the depth of each groove is 0.7mm, and the thickness of the polishing pad is 2.5 mm. The thickness of the top layer of the detection window is 0.5mm, the thickness of the middle layer is 1.7mm, and the thickness of the bottom layer is 0.3 mm. The obtained chemical mechanical polishing pad was subjected to polishing test and various physical property tests.
Example 3
The preparation method of the window comprises the following steps: the top layer and the bottom layer of the window are selected from 308g of prepolymer (PET 95A manufactured by Coim company) and 110g of MOCA (Shanghai Kaiyin), and are stirred and mixed uniformly; the interlayer material was selected from 234g of naphthalene diisocyanate (Wanhua) and 235g of pentaerythritol tetramercaptoacetate (Carxing Correct chemical). The gel time of the top/bottom layer material was tested to be 8min and the gel time of the middle layer was 11 min. Uniformly mixing the top layer material, pouring into a mold, starting timing, beginning to continue pouring the middle layer material after 4min, pouring the bottom layer material after 7min, putting the poured window into a 100 ℃ temperature, heating and curing for 8h, cooling and demolding to obtain a window block, and cutting the obtained window block into a proper size to be installed in a polishing pad.
The preparation method of the polishing pad comprises the following steps: 2876g of prepolymer (PET 95A of Coim company) and 125g of microspheres (Nobel chemical 40D25) are uniformly stirred and mixed, 1230g of curing agent MOCA (Shanghai Keyin) is added and uniformly stirred, the mixture is injected into a mold and heated to 100 ℃ for 8 hours, and the polishing layer is obtained after slicing. The polishing layer sheet was sequentially attached to a SUBA IV buffer layer (DOW) via PSA3000(3M) to obtain a polishing pad. A window sized hole was punched in the pad using a die and the window block was affixed in the pad hole by hot melt AM158 (Howtec).
The chemical mechanical polishing pad with the detection window is prepared by the method, and concentric circular grooves are engraved on the surface of the polishing pad, wherein the depth of each groove is 0.5mm, and the thickness of the polishing pad is 2.0 mm. The thickness of the top layer of the detection window is 0.5mm, the thickness of the middle layer is 1.4mm, and the thickness of the bottom layer is 0.1 mm. The obtained chemical mechanical polishing pad was subjected to polishing test and various physical property tests.
Example 4
The preparation method of the window comprises the following steps: the top and bottom layers were made of a material selected from 295g LFG963A (Kemey), and 13g ethylene glycol (Aladdin) by mixing and stirring; the interlayer material was selected from 214g of 4, 4' -dicyclohexylmethane diisocyanate (Wawa) and 230g of trimethylolethane tris (3-mercaptopropionate) (Dickins chemical). The gel time of the top/bottom layer material was tested to be 6min and the gel time of the middle layer 12 min. Uniformly mixing the top layer material, pouring into a mold, starting timing, beginning to continue pouring the middle layer material after 3min, pouring the bottom layer material after 9min, putting the poured window into a 100 ℃ heating and curing device for 8h, cooling and demolding to obtain a window block, and cutting the obtained window block into a proper size to be installed in a polishing pad.
The preparation method of the polishing pad comprises the following steps: 2568g of LFG963A (Kyobo Co.) and 99g of microspheres (Nobel chemical 40D42) were mixed by stirring, 132g of curing agent ethylene glycol (Aladdin) was added and stirred uniformly, the mixture was poured into a mold and heated to 100 ℃ for 8 hours, and the polished layer was obtained after slicing. The polishing layer sheet was sequentially attached to a SUBA IV buffer layer (DOW) via PSA3000(3M) to obtain a polishing pad. A window sized hole was punched in the pad using a die and the window block was affixed in the pad hole by hot melt AM158 (Howtec).
The chemical mechanical polishing pad with the detection window is prepared by the method, and concentric circular grooves are engraved on the surface of the polishing pad, wherein the depth of each groove is 0.5mm, and the thickness of the polishing pad is 2.1 mm. The thickness of the top layer of the detection window is 0.5mm, the thickness of the middle layer is 1.5mm, and the thickness of the bottom layer is 0.1 mm. The obtained chemical mechanical polishing pad was subjected to polishing test and various physical property tests.
Example 5
The preparation method of the window comprises the following steps: the window top and bottom layers were made of a material selected from the group consisting of 301g LF750D (Kemeyer corporation), and 47g tripropylene glycol (Alatin) and mixed together; the interlayer material was selected from 227g of isophorone diisocyanate (Wawa) (Vawa) and 257g of pentaerythritol tetrakis (3-mercaptopropionate) (Jingbo). The top/bottom layer material was tested for 13min gel time and the middle layer for 7min gel time. Uniformly mixing the top layer material, pouring into a mold, timing, continuously pouring the middle layer material after 9min, pouring the bottom layer material after 5min, putting the poured window into a mold, heating and curing at 100 ℃ for 8h, cooling and demolding to obtain a window block, and cutting the obtained window block into a proper size to be installed in a polishing pad.
The preparation method of the polishing pad comprises the following steps: 2374g of LF750D (Korea) and 137g of microspheres (Nobel chemical 40D42) were mixed and stirred uniformly, then 452g of curing agent tripropylene glycol (avadin) was added and stirred uniformly, the mixture was poured into a mold and heated to 100 ℃ for 8 hours, and the polishing layer was obtained after slicing. The polishing layer sheet was sequentially attached to a SUBA IV buffer layer (DOW) via PSA3000(3M) to obtain a polishing pad. A window sized hole was punched in the pad using a die and the window block was affixed in the pad hole by hot melt AM158 (Howtec).
The chemical mechanical polishing pad with the detection window is prepared by the method, and concentric circular grooves are engraved on the surface of the polishing pad, wherein the depth of each groove is 0.5mm, and the thickness of the polishing pad is 2.2 mm. The thickness of the top layer of the detection window is 0.5mm, the thickness of the middle layer is 1.6mm, and the thickness of the bottom layer is 0.1 mm. The obtained chemical mechanical polishing pad was subjected to polishing test and various physical property tests.
Comparative example 1
A chemical mechanical polishing pad was prepared in the same manner as in example 1, wherein the window was replaced with a single layer structure, 650g of prepolymer (PET 95A, Coim) and 220g of moca (shanghai kaien) were stirred, mixed, poured into a mold, and the pouring was stopped until the thickness reached 2.3mm, and the obtained window block was cut into a suitable size and mounted in the polishing pad. Wherein the surface of the polishing pad is carved with concentric circular grooves with the depth of 0.8 mm. The thickness of the polishing layer was 2.3 mm. The obtained chemical mechanical polishing pad was subjected to polishing test and various physical property tests.
Comparative example 2
A chemical mechanical polishing pad was obtained in the same manner as in example 1, except that the window was replaced with a single-layer structure, 572g of toluene diisocyanate (warfarin) and 840g of pentaerythritol tetrakis (3-mercaptopropionate) (kyobo) were stirred, mixed, poured into a mold, and the pouring was stopped until the thickness reached 2.3mm, and the obtained window block was cut into an appropriate size and mounted in the polishing pad. The surface of the polishing pad is carved with concentric circular grooves with the depth of 0.8 mm. The thickness of the polishing pad was 2.3 mm. The obtained chemical mechanical polishing pad was subjected to polishing test and various physical property tests.
Comparative example 3
A chemical mechanical polishing pad was obtained in the same manner as in example 1. The window top layer material is selected from 325g of prepolymer (PET 95A manufactured by Coim company) and 110g of MOCA (Shanghai Kaiyin), and is stirred and mixed uniformly; the middle layer material was selected from 286g of toluene diisocyanate (Wawa) and 420g of pentaerythritol tetrakis (3-mercaptopropionate) (Jingbo). The gel time of the top layer material was tested to be 8min and the gel time of the middle layer 8 min. Uniformly mixing the top layer material, pouring the top layer material into a mold, starting timing, beginning to continue pouring the intermediate layer material after 6min, putting the poured window into a 100 ℃ temperature, heating and curing for 8h, cooling and demolding to obtain a window block, and cutting the obtained window block into a proper size to be installed in a polishing pad.
The surface of the polishing pad is carved with concentric circular grooves, the depth of the grooves is 0.8mm, and the thickness of the polishing pad is 2.3 mm. The detection window has a two-layer structure, the thickness of the top layer of the detection window is 0.45mm, and the thickness of the middle layer is 1.65 mm. The obtained chemical mechanical polishing pad was subjected to polishing test and various physical property tests.
Comparative example 4
A chemical mechanical polishing pad was obtained in the same manner as in example 1. The window bottom layer material is selected from 325g prepolymer (PET 95A manufactured by Coim company) and 110g MOCA (Shanghai Kaiyin), and is stirred and mixed uniformly; the middle layer material was selected from 286g of toluene diisocyanate (Wawa) and 420g of pentaerythritol tetrakis (3-mercaptopropionate) (Jingbo). The gel time of the bottom layer material is 8min, and the gel time of the middle layer is 8 min. Uniformly mixing the intermediate layer materials, pouring the mixture into a mold, starting timing, pouring the bottom layer material after 6min, putting the poured window into a 100 ℃ temperature, heating and curing for 8h, cooling and demolding to obtain a window block, and cutting the obtained window block into a proper size to be installed in a polishing pad.
The surface of the polishing pad is carved with concentric circular grooves, the depth of the grooves is 0.8mm, and the thickness of the polishing pad is 2.3 mm. The detection window has a two-layer structure, the original middle layer is changed into a top layer which is a high-refractive-index layer, the thickness of the top layer is 1.65mm, and the thickness of the bottom layer is 0.2 mm. The obtained chemical mechanical polishing pad was subjected to polishing test and various physical property tests.
Comparative example 5
A chemical mechanical polishing pad was obtained in the same manner as in example 1. The preparation method of the window comprises the following steps: the top layer and the bottom layer of the window are selected from 325g of prepolymer (PET 95A manufactured by Coim company) and 110g of MOCA (Shanghai Kaiyin), and are stirred and mixed uniformly; the middle layer material was selected from 286g of toluene diisocyanate (Wawa) and 420g of pentaerythritol tetrakis (3-mercaptopropionate) (Jingbo). The gel time of the top/bottom layer material was tested to be 8min and the gel time of the middle layer 8 min. And uniformly mixing the top layer material, pouring into a mold, starting timing, continuing to pour the middle layer material after 2min, pouring the bottom layer material after 2min, putting the poured window at the temperature of 100 ℃ for heating and curing for 8h, cooling and demolding to obtain a window block.
The surface of the polishing pad is engraved with concentric circular grooves, the depth of the grooves is 0.8mm, and the thickness of the polishing pad is 2.3 mm. The thickness of the top layer of the detection window is 0.45mm, the thickness of the middle layer is 1.65mm, and the thickness of the bottom layer is 0.2 mm. The obtained chemical mechanical polishing pad was subjected to polishing test and various physical property tests.
Comparative example 6
A chemical mechanical polishing pad was obtained in the same manner as in example 1. The preparation method of the window comprises the following steps: the top layer and the bottom layer of the window are selected from 325g of prepolymer (PET 95A manufactured by Coim company) and 110g of MOCA (Shanghai Kaiyin), and are stirred and mixed uniformly; the middle layer material was selected from 286g of toluene diisocyanate (Wawa) and 420g of pentaerythritol tetrakis (3-mercaptopropionate) (Jingbo). The gel time of the top/bottom layer material was tested to be 8min and the gel time of the middle layer 8 min. And uniformly mixing the top layer material, pouring into a mold, starting timing, continuing pouring the intermediate layer material after 12min, pouring the bottom layer material after 15min, heating and curing the poured window at 100 ℃ for 8h, cooling and demolding to obtain a window block.
The surface of the polishing pad is engraved with concentric circular grooves, the depth of the grooves is 0.8mm, and the thickness of the polishing pad is 2.3 mm. The thickness of the top layer of the detection window is 0.45mm, the thickness of the middle layer is 1.65mm, and the thickness of the bottom layer is 0.2 mm. The obtained chemical mechanical polishing pad was subjected to polishing test and various physical property tests.
Comparative example 7
A chemical mechanical polishing pad was obtained in the same manner as in example 1. The preparation method of the window comprises the following steps: the top layer and the bottom layer of the window are selected from 325g of prepolymer (PET 95A manufactured by Coim company) and 110g of MOCA (Shanghai Kaiyin), and are stirred and mixed uniformly; the interlayer material was chosen from 286g of TDI-100 (Wawa) and 258g of 1, 6-hexanedithiol (Tentah. Nature). The gel time of the top/bottom layer material was tested to be 8min and the gel time of the middle layer was tested to be 9 min. And uniformly mixing the top layer material, pouring into a mold, starting timing, continuously pouring the middle layer material after 6min, pouring the bottom layer material after 7min, putting the poured window at the temperature of 100 ℃, heating and curing for 8h, cooling and demolding to obtain a window block.
The chemical mechanical polishing pad with the detection window is prepared by the method, and concentric circular grooves are engraved on the surface of the polishing pad, wherein the depth of each groove is 0.8mm, and the thickness of the polishing pad is 2.3 mm. The thickness of the top layer of the detection window is 0.45mm, the thickness of the middle layer is 1.65mm, and the thickness of the bottom layer is 0.2 mm. The obtained chemical mechanical polishing pad was subjected to polishing test and various physical property tests.
The polishing pads of the examples and comparative examples were subjected to polishing experiments and performance tests using the methods described previously, and the data obtained are shown in table one.
TABLE 1 test results data sheet
Figure BDA0003382180140000171
As can be seen from the data in the table, the polishing pads prepared by the method of the present invention in the examples exhibited significantly reduced scratches on the wafer surface after the polishing test. The detection window has high initial refractive index, and simultaneously, as the top layer of the detection window with a sandwich-like structure is continuously worn, the volume ratio of the middle layer to the detection window is increased, so that the integral refractive index of the detection window is increased at the later stage of polishing, the reflection intensity of incident light is reduced, and the accuracy of end point detection is improved.
In comparative example 1, where a polishing pad structure having a conventional refractive index window was used, although the degree of scratching of the wafer surface after polishing was not so great, the refractive index of the detection window was low, indicating that a large amount of incident detection light was scattered off the bottom surface of the detection window, affecting the accuracy of the detection of the polishing endpoint. The detection window in comparative example 2 is made of a high-refraction material, the polymer has a low compression rate, and deformation occurring in the polishing process is different from the deformation occurring in the polishing pad, so that the surface of the wafer is more easily scratched. The detection window in comparative examples 1 and 2 was of a single structure type, and there was no significant change in the refractive index of the detection window before and after polishing. Comparative example 3 the detection window does not have a bottom layer structure, so that the high refractive index layer as a "base" bears the pressure and deformation during the whole polishing process, and compared with the polishing pad, the detection window cannot make a timely stress-strain response, and the number of scratches is increased. However, similar to the embodiment, as the polishing progresses, the top layer structure is continuously worn, so that the overall refractive index of the detection window is improved after the polishing is finished. In comparative example 4, the high refractive index layer directly contacts the surface of the wafer, the number of scratches increases due to the different polishing characteristics from the polishing layer, and the final refractive index of the inspection window decreases as the high refractive index layer wears down during the polishing process. In the comparative example 5, the interval time of each layer is short in the pouring process of the sandwich structure, good layering is not formed, partial chains in the window are arranged in a disordered way, the refractive index of the detection window is influenced, and the refractive index of the detection window does not change obviously along with the polishing process. Comparative example 6 little or no chemical bonding between layers was formed during the casting of the "sandwich" structure, the bonding between layers was not tight and the risk of delamination was easily observed, and for the same reason, the refractive index of the test window increased as the top layer was worn away as polishing proceeded. Compared with the window intermediate layer in the step 7 which uses difunctional mercaptan, compared with trifunctional mercaptan, the obtained window has lower refractive index, reduces the optical detection accuracy and is more prone to generate polishing defects.
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. It will be appreciated by those skilled in the art that modifications or adaptations to the invention may be made in light of the teachings of the present specification. Such modifications or adaptations are intended to be within the scope of the present invention as defined in the claims.

Claims (10)

1. A chemical mechanical polishing pad with high end point detection precision comprises a polishing layer and a detection window, and is characterized in that the detection window has a sandwich-like structure of a top layer, a middle layer and a bottom layer facing a polishing surface, and the thickness of the detection window is the same as that of the polishing pad; the top layer and the bottom layer are made of the same material and both are made of a polymer matrix material, and the middle layer is made of a high-refractive-index material containing a thiol compound.
2. The chemical mechanical polishing pad according to claim 1, wherein the thiol compound contained in the high refractive index material of the intermediate layer is a thiol compound having at least three mercapto groups; preferably, the refractive index of the whole detection window ranges from 1.55 to 1.67.
3. The chemical mechanical polishing pad of claim 1 or 2, wherein the polishing layer is comprised of a polymeric matrix material and polymeric microelements; preferably, the polymer matrix material is a thermosetting material, more preferably a polyurethane material, and the polymeric microelements are microspheres; further preferably, the addition amount of the microspheres accounts for 2-5 wt% of the total mass of the polyurethane.
4. The chemical mechanical polishing pad according to any one of claims 1 to 3, wherein the surface of the polishing layer has macro-structured grooves having a depth of 0.5 to 0.8 mm; preferably, the thickness of the top layer of the detection window is greater than or equal to 1/2 of the groove depth of the polishing layer and less than or equal to the groove depth; more preferably, the thickness of the bottom layer of the detection window is greater than 0mm and less than 0.5 mm.
5. The chemical mechanical polishing pad of any one of claims 1-4, wherein the detection window has a Shore D hardness on the surface that is within ± 5D of the Shore D hardness on the surface of the polishing layer; preferably, the compression ratio of the detection window is within ± 0.5% of the compression ratio of the polishing layer.
6. The chemical mechanical polishing pad according to any one of claims 1 to 5, further comprising an adhesive layer and a buffer layer, wherein the polishing layer and the buffer layer are attached by the adhesive layer, wherein the adhesive layer is selected from one or a combination of a pressure sensitive adhesive and a hot melt adhesive, and the buffer layer is selected from a polyurethane felt-type or foam-type structure layer.
7. The method for preparing a chemical mechanical polishing pad according to any one of claims 1 to 6, comprising the steps of preparing the following detection windows:
1) from NCO group-containing prepolymers and NH-containing prepolymers2Or OH, and pouring a top layer structure of the detection window, wherein the gel time of the top layer structure is t1，t15-15 min; preferably, wherein NCO is reacted with unreacted NH2Or the molar ratio of OH is 1-1.2;
2) by reaction of isocyanates with thiol compounds at t1-4～t1-casting an intermediate layer structure of the detection window within 2min, the intermediate layer structure having a gel time t2，t25-13 min; preferably, the molar ratio of NCO in isocyanate to SH in thiol compound is 0.9-1.1;
3) from NCO group-containing prepolymers and NH-containing prepolymers2Or OH, at t2-4～t2-casting the substructure within 2 min; preferably, wherein NCO is reacted with unreacted NH2Or the molar ratio of OH is 1-1.2;
preferably, the detection window is prepared by sequentially pouring and molding from step 1) to step 3) from bottom to top or from top to bottom.
8. The method of claim 7, further comprising a step of preparing a polishing layer composed of a prepolymer containing NCO groups and a prepolymer containing NH groups2Or OH curing agent and microsphere curing reaction; preferably, unreacted NH in the polishing layer2Or the molar ratio of OH to NCO is 0.8-1; more preferably, in the polishing layer, the addition amount of the microspheres is 2-5 wt% of the total mass of the polyurethane.
9. The method of claim 8, wherein the detection window is formed in the same mold, and the polishing layer is formed to form a polishing pad of the integrated window; or preparing the detection window and the polishing layer respectively, then opening a hole on the polishing layer and inserting the detection window to obtain the polishing pad with the insertion-type detection window.
10. Use of the chemical mechanical polishing pad according to any one of claims 1 to 6 or the chemical mechanical polishing pad produced by the production method according to any one of claims 8 to 9 for chemical mechanical polishing of a magnetic substrate, an optical substrate or a semiconductor substrate.
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