A composite abrasive particle polishing pad containing a shear thickening fluid, method of manufacture and use
By using a composite abrasive polishing pad with shear-thickening fluid in SiC material polishing, combined with abrasives of different particle sizes and a polyurethane microporous framework, efficient and precise polishing of SiC materials has been achieved, solving the problems of low polishing efficiency and poor quality of SiC materials, and improving processing efficiency and accuracy.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- QUZHOU BOLAINARUN ELECTRONIC MATERIALS CO LTD
- Filing Date
- 2024-05-15
- Publication Date
- 2026-06-19
AI Technical Summary
Existing chemical mechanical polishing processes for SiC materials suffer from low polishing efficiency, subsurface damage, and poor surface quality. In particular, in the polishing of free abrasives and bonded abrasives, the unstable dispersion and uneven wear of the abrasives lead to poor processing quality.
A composite abrasive polishing pad containing a shear-thickening fluid is used. By compounding silica aqueous solution and single-crystal diamond abrasives in a polyurethane soft microporous skeleton, the rheological properties of the shear-thickening fluid are utilized to achieve a semi-consolidated state of the abrasives during the polishing process. This enhances the holding effect of the abrasives and improves the uniformity of surface stress. Combined with equipment control, high removal rate and high-precision polishing are achieved.
It improves the polishing efficiency and precision of SiC materials, simplifies the process steps, enhances processing efficiency and accuracy, and solves the problems of surface roughness and damage of SiC materials.
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Figure CN118288193B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of polishing technology, and in particular to a composite abrasive polishing pad containing a shear-thickening fluid, its preparation method, and its application. Background Technology
[0002] Currently, the main processing steps for SiC materials include: directional dicing, rough grinding, fine grinding, mechanical polishing, and chemical mechanical polishing (CMP). Among these, CMP, as the final step, directly impacts polishing efficiency and processing costs through the selection of process methods, process route layout, and optimization of process parameters. In the semiconductor field, achieving an ultra-smooth, defect-free, and damage-free surface on SiC single wafers after CMP is a decisive factor in the growth of high-quality epitaxial layers. In the field of optical mirrors, CMP technology influences the competitive advantage and development momentum of SiC materials in optical mirror applications, serving as a fundamental path to reduce surface roughness, minimize scattering losses, and obtain optical surfaces. In the field of mechanical seals, CMP is a novel measure to reduce surface roughness, enhance the sealing performance of SiC as a hydrodynamic component, and prevent leakage. Traditional CMP for SiC can be categorized based on the abrasive's state: free abrasive polishing, bonded abrasive polishing, and semi-bonded abrasive polishing.
[0003] The free abrasive polishing apparatus mainly consists of three parts: a rotary table, a specimen clamping device, and a polishing slurry delivery device. A polishing pad is attached to the rotary table and rotates on its own. An external support applies positive pressure to the wafer, creating a suitable positive pressure between the wafer and the polishing pad, enabling relative motion. Material removal is achieved through a three-body friction method; that is, when the abrasive is between the specimen surface and the polishing pad surface, the two surfaces and the abrasive form a three-body structure. This chemical mechanical polishing method involves many process parameters. Issues such as the dispersion instability of the free abrasive and the clogging of the polishing pad's micropores by the free abrasive leading to glazing ultimately affect the SiC material removal rate and surface quality (subsurface damage).
[0004] Due to the shortcomings of free abrasive chemical mechanical polishing (CMP) and the ever-increasing demands for wafer planarization, bonded abrasive polishing technology emerged. In this process, the abrasive is bonded within the polishing pad, and the polishing slurry no longer contains abrasive but rather an aqueous solution or deionized water containing only basic chemical components. External pressure can be directly applied to the abrasive, and the wafer is held by a fixture, with the abrasive and polishing pad fixed together, restricting the movement of the abrasive. Using a two-body polishing method, there is relative sliding between the abrasive and the wafer during polishing. However, with a polishing pad featuring evenly distributed bonded abrasive protrusions, the density of the movement trajectory formed by the SiC wafer on the polishing pad is inconsistent, resulting in uneven wear and surface deterioration of the polishing pad, thus affecting the surface shape and subsurface quality of the SiC.
[0005] Semi-bonded abrasive polishing pads and semi-bonded abrasive machining technology utilize the "trap" effect to reduce or even eliminate surface damage caused by large particles in the abrasive grains or those intruding from the outside, thereby achieving efficient and precise machining. In semi-bonded abrasives, because the bonding force between abrasive grains is smaller than that in rigid bonded abrasive polishing pads, when large abrasive grains or large particles from the outside enter the machining area, the large grains will shift due to the weak bonding force, forming trap spaces. This causes abrasive grains of different sizes to tend to be at the same height on the polishing pad surface, thus achieving ultra-precision machining of the workpiece.
[0006] Regarding abrasives, diamond abrasives can remove more atoms when polishing silicon carbide surfaces, but they have a significant impact on the surface quality of silicon carbide workpieces. Silica abrasives primarily remove atoms through chemical reactions, resulting in lower surface atom removal efficiency, but they have virtually no impact on the surface quality of silicon carbide workpieces. In actual production, there are high requirements for both the processing efficiency and quality of silicon carbide wafers, and neither diamond nor silica abrasives alone can adequately meet these requirements. A hybrid polishing process using both types of abrasives is employed. Diamond efficiently removes large areas of unevenness on the silicon carbide surface, while silica improves the surface quality, thus ensuring both high polishing efficiency and good polishing quality.
[0007] Patent CN 110193777 A relates to the field of grinding, and particularly to a grinding pad. The grinding pad includes a pad body and a filler, the filler comprising an adhesive and abrasive particles; the adhesive is made of a viscoelastic material, and the filler is at least partially attached to the pad body. Compared to existing technologies, utilizing a viscoelastic material to bind the abrasive particles and setting the mixed filler on the pad body of the grinding pad combines the advantages of fixed abrasive grinding and free abrasive grinding, improving processing efficiency, reducing damage to the workpiece surface, and improving grinding accuracy.
[0008] The industry suffers from common problems such as low polishing efficiency, silicon carbide subsurface damage, and poor surface quality during the CMP stage of silicon carbide substrate materials. The technical requirements to be met are now more stringent, including surface roughness, removal rate, and surface shape requirements. Summary of the Invention
[0009] To solve the above-mentioned technical problems, the present invention provides a composite abrasive polishing pad containing a shear-thickening fluid, wherein the polishing pad is composed of a polyurethane soft microporous skeleton, a shear-thickening fluid, and composite abrasive.
[0010] The density of the polyurethane soft microporous skeleton is 0.10-0.20 g / cm³. 3 Thickness 2.50±0.5mm, average pore size 200±50μm;
[0011] The composite abrasive is made by combining an aqueous solution of silica and single-crystal diamond.
[0012] In one embodiment of the present invention, the particle size of the silica in the silica aqueous solution is 150-300 nm.
[0013] In one embodiment of the present invention, the particle size of the single crystal diamond is 500-1000 nm.
[0014] In one embodiment of the present invention, the mass ratio of the silica aqueous solution to single crystal diamond is 5:1 to 1:5.
[0015] In one embodiment of the present invention, the raw materials for preparing the polyurethane soft microporous framework include: polyurethane prepolymer, deionized water, polytetrahydrofuran diol, 3,3'-dichloro-4,4'-diphenylmethane diamine, a mixture of triethylenediamine and polyol, and an organosilicon surfactant. In another embodiment of the present invention, the hardness of the polyurethane prepolymer is 73-75 Shore D.
[0016] In one embodiment of the present invention, the silica aqueous solution is a silane-modified silica aqueous solution.
[0017] In one embodiment of the present invention, the raw materials for preparing the shear-thickening fluid include triethanolamine, anionic surfactant, hydroxypropyl polydimethylsiloxane, and deionized water.
[0018] A second aspect of this invention provides a method for preparing the composite abrasive polishing pad containing the shear-thickening fluid, comprising the following steps:
[0019] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran diol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine and polyol mixture and organosilicon surfactant according to the mass fractions;
[0020] SO2 polyurethane prepolymer and polytetrahydrofuran diol were mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and polyol mixture and organosilicon surfactant were mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine was kept at 120°C to form material tank C.
[0021] The raw materials from tanks A, C, and S of S03 are mixed and discharged simultaneously at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm that is kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0022] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0023] S05 The sample block was sliced, and the thickness of the polyurethane microporous skeleton after slicing was 2.50mm±0.05mm;
[0024] S06 Weigh out the following components by mass: silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, triethanolamine. Mix the silica aqueous solution and single crystal diamond at high speed of 2000-2500 rpm. Then add triethanolamine, polycarboxylic acid anionic surfactant, hydroxypropyl polydimethylsiloxane, and deionized water in sequence and mix at 1500 rpm to obtain a shear-thickened slurry.
[0025] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0026] The third aspect of the present invention provides a composite abrasive polishing pad containing shear-thickening fluid, which is applied in the field of SiC material processing.
[0027] By adopting the above technical solution, the present invention has the following beneficial effects:
[0028] In this invention, a shear-thickening fluid is prepared by combining diamond and silica abrasives of different sizes as the dispersed phase and then molded into a soft polyurethane microporous framework. The resulting composite polishing pad exhibits characteristics of both bonded and semi-bonded abrasive polishing pads, primarily achieved through the rheological properties of the shear-thickening fluid. Under equilibrium conditions, the dispersion system exhibits good fluidity; however, when the shear force exceeds its critical force, the viscosity of the dispersion system increases sharply, leading to shear thickening and a solid-like state. Once the shear force disappears, it quickly returns to a flowable state. The harder diamond abrasives and silane-modified silica abrasives withstand more stress in the shear-thickening fluid, maintaining a higher viscosity. The polishing fluid itself only requires an aqueous solution containing an oxidant. During the polishing process, when normal pressure is applied, the polishing pad, under shear force, experiences a shear thickening and expansion effect in the contact area with the workpiece, exhibiting an expansion and extrusion phenomenon. This enhances the polishing pad's grip on the abrasive grains while improving the uniformity of force on the workpiece surface. The abrasive grains in the grinding wheel, which have a polishing effect, produce a micro-cutting action on the workpiece surface, achieving material removal and polishing. Furthermore, by controlling the pressure, rotation speed, and polishing fluid flow rate of the equipment during polishing, the rheological properties of this composite polishing pad exhibit varying degrees of hardness, resilience, and impact resistance, thus achieving high removal rates and high-precision polishing of silicon carbide wafers. This simplifies the grinding and polishing process, improving processing efficiency and accuracy. Attached Figure Description
[0029] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.
[0030] Figure 1 This is a finished product image of the composite polishing pad from Example 1;
[0031] Figure 2 This is a scanning electron microscope image of the microporous soft polyurethane skeleton of Example 1;
[0032] Figure 3 This is a schematic diagram of the structure of a shear-thickened composite abrasive polishing pad. Detailed Implementation
[0033] The technical solution of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0034] The present invention provides a composite abrasive polishing pad containing a shear-thickening fluid, wherein the polishing pad is composed of a polyurethane soft microporous skeleton, a shear-thickening fluid, and composite abrasive.
[0035] The density of the polyurethane soft microporous skeleton is 0.10-0.20 g / cm³. 3 Thickness 2.50±0.5mm, average pore size 200±50μm;
[0036] The composite abrasive is made by combining an aqueous solution of silica and single-crystal diamond.
[0037] Polyurethane soft microporous skeleton
[0038] The raw materials for preparing the polyurethane soft microporous framework include: polyurethane prepolymer, deionized water, polytetrahydrofuran diol, 3,3'-dichloro-4,4'-diphenylmethane diamine, a mixture of triethylenediamine and polyol, and organosilicon surfactant.
[0039] Specifically, according to parts by weight, the raw materials for preparing the polyurethane flexible microporous framework include:
[0040] 100 parts of polyurethane prepolymer
[0041] 1-2 parts deionized water
[0042] 5-8 parts of polytetrahydrofuran diol
[0043] 5-8 parts of 3,3'-dichloro-4,4'-diphenylmethanediamine
[0044] 0.03-0.06 parts of a mixture of triethylenediamine and polyol
[0045] 1-3 parts of organosilicon surfactant.
[0046] The polyurethane prepolymer has a hardness of 73-75 Shore D and an isocyanate group content (NCO%) of 9.4-9.7%; the polytetrahydrofuran diol has a molecular weight of 2000.
[0047] The polyol in the triethylenediamine and polyol mixture can be selected from one or more of dipropylene glycol, ethylene glycol, and 1,4-butanediol, and the content of triethylenediamine in the mixture is 33%.
[0048] In this invention, the density of the polyurethane flexible microporous skeleton is 0.10-0.20 g / cm³. 3 The thickness is 2.50±0.5mm, the average pore size is 200±50μm, and the diameter of the finished polishing pad is 950mm.
[0049] It consists of 1-3 parts of silicone surfactant (Niax L-1501 from Momentive, TEGOSTAB 8948 from Evonik, DABCO PE 40, or DC-193 from Dow).
[0050] Shear-thickening fluid
[0051] In this invention, the raw materials for preparing the shear-thickening fluid include: 2-5 parts triethanolamine, 0.2-1 parts polycarboxylic acid anionic surfactant, 1-5 parts hydroxypropyl polydimethylsiloxane, and 20-50 parts deionized water.
[0052] In this invention, the polycarboxylic acid anionic surfactant is Dow Duramax D-205, and the hydroxypropyl polydimethylsiloxane is Dow... HY-3050.
[0053] In a preferred embodiment of the present invention, the raw materials for preparing the shear-thickening fluid further include Dow Tergitol-TMN-10; and the mass ratio of Tergitol-TMN-10 to the polycarboxylic acid anionic surfactant is 1:5.
[0054] Composite abrasives
[0055] In this invention, the composite abrasive is composed of an aqueous silica solution and single-crystal diamond; and the aqueous silica solution is a silane-modified silica solution (solid content 50%), wherein the silica particle size in the aqueous silica solution is 150-300 nm; the single-crystal diamond is selected with a particle size of 500-1000 nm; preferably, the mass ratio of the silica solution to single-crystal diamond particles is 5:1 to 1:5.
[0056] The silane-modified silica aqueous solution described in this invention is (Shanghai Yingzhi Abrasive Materials Co., Ltd. YZ828M).
[0057] This patent first controls the particle size and mixing ratio of two special functional abrasives, diamond and functionalized silica, to achieve controllable dispersion in a shear-thickening fluid medium. Then, a specially structured polyurethane foam soft skeleton is prepared in a one-step process, organically combining the two. The abrasives, aided by the shear-thickening fluid, selectively concentrate within the polyurethane foam soft skeleton matrix, forming a microphase-separated composite polishing pad structure. During CMP, the composite polishing pad's responsiveness to temperature and pressure causes a sharp increase in the viscosity of the internal microphase-separated components. The mixed abrasives exhibit a semi-solidified state on the polishing pad surface, creating a "trap" effect during polishing. This effect improves the quality of precision machining of silicon carbide substrates.
[0058] The free hydroxyl radicals (·OH) generated by the thermal catalysis of the hydroxyl surfactant in the polishing pad and the oxidant in the polishing slurry undergo a solid-phase reaction with the silicon carbide substrate, forming an easily removable soft SiO2 oxide layer on the substrate surface, greatly improving processing efficiency. The different surface energies of the diamond particles and modified silica particles result in their concentrated distribution on the polishing pad surface, but with different solidification states. When polishing under higher pressure, diamond abrasive particles play a major grinding role, increasing the removal rate; when polishing under lower pressure, modified silica abrasive particles play a major grinding role, improving the surface quality of the silicon carbide. This results in superior technical performance.
[0059] In this invention, a shear-thickening fluid is prepared by combining diamond and silica abrasives of different sizes as the dispersed phase and then molded into a soft polyurethane microporous framework. The resulting composite polishing pad exhibits characteristics of both bonded and semi-bonded abrasive polishing pads, primarily achieved through the rheological properties of the shear-thickening fluid. Under equilibrium conditions, the dispersion system exhibits good fluidity; however, when the shear force exceeds its critical force, the viscosity of the dispersion system increases sharply, leading to shear thickening and a solid-like state. Once the shear force disappears, it quickly returns to a flowable state. The harder diamond abrasives and silane-modified silica abrasives withstand more stress in the shear-thickening fluid, maintaining a higher viscosity. The polishing fluid itself only requires an aqueous solution containing an oxidant. During the polishing process, when normal pressure is applied, the polishing pad, under shear force, experiences a shear thickening and expansion effect in the contact area with the workpiece, exhibiting an expansion and extrusion phenomenon. This enhances the polishing pad's grip on the abrasive grains while improving the uniformity of force on the workpiece surface. The abrasive grains in the grinding wheel, which have a polishing effect, produce a micro-cutting action on the workpiece surface, achieving material removal and polishing. Furthermore, by controlling the pressure, rotation speed, and polishing fluid flow rate of the equipment during polishing, the rheological properties of this composite polishing pad exhibit varying degrees of hardness, resilience, and impact resistance, thus achieving high removal rates and high-precision polishing of silicon carbide wafers. This simplifies the grinding and polishing process, improving processing efficiency and accuracy.
[0060] The present invention will be further explained below with reference to specific embodiments.
[0061] Example 1
[0062] The raw material for the polyurethane soft microporous framework consists of 100 parts of 75D polyurethane prepolymer (Covestro, Germany). The composition includes: LU-T75D isocyanate group content (NCO%) 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol solution (Momentive Niax A-33, USA); and 1.5 parts silicone surfactant (Momentive Niax L-1501 and Evonik TEGOSTAB 8948 in a mass ratio of 2:1).
[0063] The shear thickening fluid is composed of 100 parts silica: 300nm silane-modified silica aqueous solution (50% solid content) with a mass ratio of silica to single crystal diamond of 3:1, 500nm single crystal diamond, 2 parts triethanolamine, 0.5 parts Dow Duramax D-205, 0.1 parts Dow Tergitol-TMN-10, 5 parts hydroxypropyl polydimethylsiloxane, and deionized water with a particle ratio of 0.2.
[0064] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0065] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0066] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0067] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0068] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0069] S06 Weigh out the following components by mass: silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine. First, mix the silica aqueous solution and single crystal diamond at high speed (2000-2500 rpm). Then, add triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, hydroxypropyl polydimethylsiloxane, and deionized water in sequence and mix at 1500 rpm to obtain a shear-thickening slurry.
[0070] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0071] Example 2
[0072] The raw material for the polyurethane soft microporous framework consists of 100 parts of 75D polyurethane prepolymer (Covestro, Germany). The composition of LU-T75D isocyanate group content (NCO%) is 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol (Momentive Niax A-33, USA); 1.5 parts silicone surfactant (Momentive Niax L-1501 and Evonik TEGOSTAB 8948 in a mass ratio of 2:1).
[0073] The shear thickening fluid is composed of 100 parts silica: 300nm silane-modified silica aqueous solution (50% solid content) in a mass ratio of 3:1 (silica:monocrystalline diamond), 500nm monocrystalline diamond, 2 parts triethanolamine, 0.5 parts Dow Duramax D-205, 0.1 parts Dow Tergitol-TMN-10, 5 parts hydroxypropyl polydimethylsiloxane, and deionized water in a particle ratio of 0.5.
[0074] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0075] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0076] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0077] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0078] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0079] S06 Weigh out the following components by mass: silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine. First, mix the silica aqueous solution and single crystal diamond at high speed (2000-2500 rpm). Then, add triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, hydroxypropyl polydimethylsiloxane, and deionized water in sequence and mix at 1500 rpm to obtain a shear-thickening slurry.
[0080] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0081] Example 3
[0082] The raw material for the polyurethane soft microporous framework consists of 100 parts of 75D polyurethane prepolymer (Covestro, Germany). The composition of LU-T75D isocyanate group content (NCO%) is 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol (Momentive Niax A-33, USA); 1.5 parts silicone surfactant (Momentive Niax L-1501 and Evonik TEGOSTAB 8948 in a mass ratio of 2:1).
[0083] The shear thickening fluid is composed of 100 parts silica: 1:1 (mass ratio of silica to single crystal diamond) of 300 nm silane-modified silica aqueous solution (50% solid content), 500 nm single crystal diamond, 2 parts triethanolamine, 0.5 parts Dow Duramax D-205, 0.1 parts Dow Tergitol-TMN-10, 5 parts hydroxypropyl polydimethylsiloxane, and deionized water with a particle ratio of 0.2.
[0084] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0085] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0086] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0087] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0088] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0089] S06 Weigh out the following components by mass: silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine. First, mix the silica aqueous solution and single crystal diamond at high speed (2000-2500 rpm). Then, add triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, hydroxypropyl polydimethylsiloxane, and deionized water in sequence and mix at 1500 rpm to obtain a shear-thickening slurry.
[0090] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0091] Example 4
[0092] The raw material for the polyurethane soft microporous framework consists of 100 parts of 75D polyurethane prepolymer (Covestro, Germany). The composition of LU-T75D isocyanate group content (NCO%) is 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol (Momentive Niax A-33, USA); 1.5 parts silicone surfactant (Momentive Niax L-1501 and Evonik TEGOSTAB 8948 in a mass ratio of 2:1).
[0093] The shear thickening fluid is composed of 100 parts silica: 1:1 (mass ratio of silica to single crystal diamond) of 300nm silane-modified silica aqueous solution (solid content 50%), 500nm single crystal diamond, 2 parts triethanolamine, 0.5 parts Dow Duramax D-205, 0.1 parts Dow Tergitol-TMN-10, 5 parts hydroxypropyl polydimethylsiloxane, and deionized water with a particle ratio of 0.5.
[0094] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0095] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0096] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0097] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0098] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0099] S06 Weigh out the following components by mass: silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine. First, mix the silica aqueous solution and single crystal diamond at high speed (2000-2500 rpm). Then, add triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, hydroxypropyl polydimethylsiloxane, and deionized water in sequence and mix at 1500 rpm to obtain a shear-thickening slurry.
[0100] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0101] Example 5
[0102] The polyurethane soft microporous framework raw material consists of 100 parts of 75D polyurethane prepolymer in a polyether / TDI system (Covestro, Germany). The composition includes: LU-T75D isocyanate group content (NCO%) 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol (Momentive Niax A-33, USA); and 1.5 parts silicone surfactant (Momentive Niax L-1501 and Evonik TEGOSTAB 8948 in a mass ratio of 2:1).
[0103] The shear thickening fluid is composed of 100 parts silica: 1 part single crystal diamond in a mass ratio of 1:3 (300 nm silane-modified silica aqueous solution (50% solid content)), 500 nm single crystal diamond, 2 parts triethanolamine, 0.5 parts Dow Duramax D-205, 0.1 parts Dow Tergitol-TMN-10, 5 parts hydroxypropyl polydimethylsiloxane, and deionized water in a particle ratio of 0.2.
[0104] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0105] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0106] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0107] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0108] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0109] S06 Weigh out the following components by mass: silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine. First, mix the silica aqueous solution and single crystal diamond at high speed (2000-2500 rpm). Then, add triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, hydroxypropyl polydimethylsiloxane, and deionized water in sequence and mix at 1500 rpm to obtain a shear-thickening slurry.
[0110] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0111] Example 6
[0112] The polyurethane soft microporous framework raw material consists of 100 parts of 75D polyurethane prepolymer in a polyether / TDI system (Covestro, Germany). The composition includes: LU-T75D isocyanate group content (NCO%) 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol (Momentive Niax A-33, USA); and 1.5 parts silicone surfactant (Momentive Niax L-1501 and Evonik TEGOSTAB 8948 in a mass ratio of 2:1).
[0113] The shear thickening fluid is composed of 100 parts silica: 1 part single crystal diamond in a mass ratio of 1:3 (300 nm silane-modified silica aqueous solution (50% solid content)), 500 nm single crystal diamond, 2 parts triethanolamine, 0.5 parts Dow Duramax D-205, 0.1 parts Dow Tergitol-TMN-10, 5 parts hydroxypropyl polydimethylsiloxane, and deionized water in a particle ratio of 0.5.
[0114] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0115] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0116] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0117] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0118] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0119] S06 Weigh out the following components by mass: silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine. First, mix the silica aqueous solution and single crystal diamond at high speed (2000-2500 rpm). Then, add triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, 5 parts of hydroxypropyl polydimethylsiloxane, and deionized water in sequence. Stir at 1500 rpm to obtain a shear-thickening slurry.
[0120] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0121] Comparative Example 1
[0122] The raw material for the polyurethane soft microporous framework consists of 100 parts of 75D polyurethane prepolymer (Covestro, Germany). The composition of LU-T75D isocyanate group content (NCO%) is 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol (Momentive Niax A-33, USA); 1.5 parts silicone surfactant (Momentive Niax L-1501 and Evonik TEGOSTAB 8948 in a mass ratio of 2:1).
[0123] The shear thickening fluid is composed of 100 parts of 300nm silane-modified silica aqueous solution (50% solid content), 2 parts of triethanolamine, 0.5 parts of Dow Duramax D-205, 0.1 parts of Dow Tergitol-TMN-10, 5 parts of hydroxypropyl polydimethylsiloxane, and deionized water in a particle ratio of 0.2.
[0124] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0125] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0126] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0127] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0128] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0129] S06 Weigh out the silica aqueous solution, deionized water, polycarboxylic acid anionic surfactant, triethanolamine, and silica aqueous solution according to the mass fractions. Then add triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, hydroxypropyl polydimethylsiloxane, and deionized water in sequence. Stir and mix at 1500 rpm to obtain a shear-thickening slurry.
[0130] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0131] Comparative Example 2
[0132] The raw material for the polyurethane soft microporous framework consists of 100 parts of 75D polyurethane prepolymer (Covestro, Germany). The composition of LU-T75D isocyanate group content (NCO%) is 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol (Momentive Niax A-33, USA); 1.5 parts silicone surfactant (Momentive Niax L-1501 and Evonik TEGOSTAB 8948 in a mass ratio of 2:1).
[0133] The shear thickening fluid is composed of 50 parts 500nm single crystal diamond, 2 parts triethanolamine, 0.5 parts Dow Duramax D-205, 0.1 parts Dow Tergitol-TMN-10, 5 parts hydroxypropyl polydimethylsiloxane, and deionized water with a particle ratio of 0.2.
[0134] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0135] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0136] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0137] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0138] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0139] S06 is weighed according to the following parts by mass: single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine. First, the single crystal diamond and deionized water are mixed at high speed of 2000-2500 rpm. Then, triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, and hydroxypropyl polydimethylsiloxane are added in sequence and mixed at 1500 rpm to obtain a shear-thickening slurry.
[0140] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0141] Comparative Example 3
[0142] The raw material for the polyurethane soft microporous framework consists of 100 parts of 75D polyurethane prepolymer (Covestro, Germany). The composition of LU-T75D isocyanate group content (NCO%) is 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol solution (Momentive Niax A-33, USA); 1.5 parts silicone surfactant (Momentive Niax L-1501, USA).
[0143] The shear thickening fluid is composed of 100 parts silica: 300nm silane-modified silica aqueous solution (50% solid content) with a mass ratio of silica to single crystal diamond of 3:1, 500nm single crystal diamond, 2 parts triethanolamine, 0.5 parts Dow Duramax D-205, 0.1 parts Dow Tergitol-TMN-10, 5 parts hydroxypropyl polydimethylsiloxane, and deionized water with a particle ratio of 0.2.
[0144] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0145] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0146] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0147] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0148] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0149] S06 Weigh out the following components by mass: silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine. First, mix the silica aqueous solution and single crystal diamond at high speed (2000-2500 rpm). Then, add triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, hydroxypropyl polydimethylsiloxane, and deionized water in sequence and mix at 1500 rpm to obtain a shear-thickening slurry.
[0150] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0151] Comparative Example 4
[0152] The raw material for the polyurethane soft microporous framework consists of 100 parts of 75D polyurethane prepolymer (Covestro, Germany). The composition includes: LU-T75D isocyanate group content (NCO%) 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol solution (Momentive Niax A-33, USA); and 1.5 parts silicone surfactant (Momentive Niax L-1501 and Evonik TEGOSTAB 8948 in a mass ratio of 2:1).
[0153] The shear thickening fluid is composed of 100 parts silica: 300nm silane-modified silica aqueous solution (50% solid content) with a mass ratio of silica to single crystal diamond of 3:1, 500nm single crystal diamond, 2 parts triethanolamine, 0.5 parts Dow Duramax D-205, 5 parts hydroxypropyl polydimethylsiloxane, and deionized water with a particle ratio of 0.2.
[0154] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0155] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0156] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0157] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0158] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0159] S06 Weigh out the following components by mass: silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine. First, mix the silica aqueous solution and single crystal diamond at high speed (2000-2500 rpm). Then, add triethanolamine, Dow Duramax D-205, hydroxypropyl polydimethylsiloxane, and deionized water in sequence and mix at 1500 rpm to obtain a shear-thickening slurry.
[0160] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0161] Comparative Example 5
[0162] The raw material for the polyurethane soft microporous framework consists of 100 parts of 75D polyurethane prepolymer (Covestro, Germany). The composition includes: LU-T75D isocyanate group content (NCO%) 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol solution (Momentive Niax A-33, USA); and 1.5 parts silicone surfactant (Momentive Niax L-1501 and Evonik TEGOSTAB 8948 in a mass ratio of 2:1).
[0163] The shear thickening fluid is composed of 100 parts silica: 300nm silica aqueous solution (50% solid content) in a mass ratio of 3:1 (silica:monocrystalline diamond), 500nm monocrystalline diamond, 2 parts triethanolamine, 0.5 parts Dow Duramax D-205, 0.1 parts Dow Tergitol-TMN-10, 5 parts hydroxypropyl polydimethylsiloxane, and deionized water in a particle ratio of 0.2.
[0164] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0165] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0166] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0167] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0168] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0169] S06 Weigh out the following components by mass: silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine. First, mix the silica aqueous solution and single crystal diamond at high speed (2000-2500 rpm). Then, add triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, hydroxypropyl polydimethylsiloxane, and deionized water in sequence and mix at 1500 rpm to obtain a shear-thickening slurry.
[0170] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0171] Comparative Example 6
[0172] The raw material for the polyurethane soft microporous framework consists of 100 parts of 75D polyurethane prepolymer (Covestro, Germany). The composition includes: LU-T75D isocyanate group content (NCO%) 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol solution (Momentive Niax A-33, USA); and 1.5 parts silicone surfactant (Momentive Niax L-1501 and Evonik TEGOSTAB 8948 in a mass ratio of 2:1).
[0173] The shear thickening fluid is composed of 100 parts of 300nm silane-modified silica and 500nm single crystal diamond in a mass ratio of silica to single crystal diamond of 1.5:1, 2 parts of triethanolamine, 0.5 parts of Dow Duramax D-205, 0.1 parts of Dow Tergitol-TMN-10, 5 parts of hydroxypropyl polydimethylsiloxane, and deionized water in a particle ratio of 0.2.
[0174] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0175] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0176] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0177] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0178] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0179] S06 Weigh out silica, monocrystalline diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine according to the mass fractions. First, mix the silica aqueous solution and monocrystalline diamond at high speed of 2000-2500 rpm. Then, add triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, hydroxypropyl polydimethylsiloxane, and deionized water in sequence and mix at 1500 rpm to obtain a shear-thickening slurry.
[0180] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0181] Comparative Example 7
[0182] The raw material for the polyurethane soft microporous framework consists of 100 parts of 75D polyurethane prepolymer (Covestro, Germany). The composition includes: LU-T75D isocyanate group content (NCO%) 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol solution (Momentive Niax A-33, USA); and 1.5 parts silicone surfactant (Momentive Niax L-1501 and Evonik TEGOSTAB 8948 in a mass ratio of 2:1).
[0183] The shear thickening fluid is composed of 100 parts silica: 3:1 mass ratio of 200nm silane-modified silica aqueous solution (50% solid content), 500nm single crystal diamond, 2 parts triethanolamine, 0.5 parts Dow Duramax D-205, 0.1 parts Dow Tergitol-TMN-10, 5 parts hydroxypropyl polydimethylsiloxane, and deionized water with a particle ratio of 0.2.
[0184] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0185] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0186] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0187] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0188] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0189] S06 Weigh out the following components by mass: silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine. First, mix the silica aqueous solution and single crystal diamond at high speed (2000-2500 rpm). Then, add triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, hydroxypropyl polydimethylsiloxane, and deionized water in sequence and mix at 1500 rpm to obtain a shear-thickening slurry.
[0190] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0191] Comparative Example 8
[0192] The raw material for the polyurethane soft microporous framework consists of 100 parts of 75D polyurethane prepolymer (Covestro, Germany). The composition includes: LU-T75D isocyanate group content (NCO%) 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% dipropylene glycol solution (Momentive Niax A-33, USA); and 1.5 parts silicone surfactant (Momentive Niax L-1501 and Evonik TEGOSTAB 8948 in a mass ratio of 2:1).
[0193] The shear thickening fluid is composed of 100 parts silica: 300nm silane-modified silica aqueous solution (50% solid content) in a mass ratio of 3:1 (silica:monocrystalline diamond), 2 parts triethanolamine, 0.5 parts Dow Duramax D-205, 0.1 parts Dow Tergitol-TMN-10, 5 parts hydroxypropyl polydimethylsiloxane, and deionized water in a particle ratio of 0.2.
[0194] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% dipropylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0195] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% dipropylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0196] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0197] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0198] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0199] S06 Weigh out the following components by mass: silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine. First, mix the silica aqueous solution and single crystal diamond at high speed (2000-2500 rpm). Then, add triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, hydroxypropyl polydimethylsiloxane, and deionized water in sequence and mix at 1500 rpm to obtain a shear-thickening slurry.
[0200] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0201] Comparative Example 9
[0202] The raw material for the polyurethane soft microporous framework consists of 100 parts of 75D polyurethane prepolymer (Covestro, Germany). The composition includes: LU-T75D isocyanate group content (NCO%) 9.5%; 1.3 parts deionized water; 7 parts polytetrahydrofuran glycol (BASF PolyTHF 2000, USA); 7 parts 3,3'-dichloro-4,4'-diphenylmethane diamine (Suzhou Xiangyuan MOCA-II type, Shandong Chongshun Hartcure M (MOCA)); 0.05 parts 33% triethylenediamine and 67% ethylene glycol solution; and 1.5 parts silicone surfactant (Niax L-1501 from Momentive, USA and Evonik TEGOSTAB 8948 from Germany in a mass ratio of 2:1).
[0203] The shear thickening fluid is composed of 100 parts silica: 300nm silane-modified silica aqueous solution (50% solid content) with a mass ratio of silica to single crystal diamond of 3:1, 500nm single crystal diamond, 2 parts triethanolamine, 0.5 parts Dow Duramax D-205, 0.1 parts Dow Tergitol-TMN-10, 5 parts hydroxypropyl polydimethylsiloxane, and deionized water with a particle ratio of 0.2.
[0204] S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran glycol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine, and 67% ethylene glycol solution and silicone surfactant according to the mass fractions. The polyurethane prepolymer and polytetrahydrofuran glycol need to be preheated at 80°C for 2 hours, and the 3,3'-dichloro-4,4'-diphenylmethane diamine needs to be heated to 120°C and kept in a molten state for later use.
[0205] SO2 polyurethane prepolymer and polytetrahydrofuran diol are first mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and 67% ethylene glycol solution and organosilicon surfactant are mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine, which is kept at 120°C, is used as material tank C.
[0206] Raw materials from tanks A, C, and S of S03 are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm and kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.2. The sample is demolded after 2 hours at 80℃.
[0207] The S04 sample block was placed in an oven and post-cured at 100°C for 16 hours to obtain a cured sample block.
[0208] S05 The sample block was sliced, and after surface finishing, the thickness of the polyurethane microporous skeleton was 2.50mm ± 0.05mm.
[0209] S06 Weigh out the following components by mass: silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine. First, mix the silica aqueous solution and single crystal diamond at high speed (2000-2500 rpm). Then, add triethanolamine, Dow Duramax D-205, Dow Tergitol-TMN-10, hydroxypropyl polydimethylsiloxane, and deionized water in sequence and mix at 1500 rpm to obtain a shear-thickening slurry.
[0210] After the bottom of the S07 polyurethane microporous skeleton sheet is flat-laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form.
[0211] Performance testing
[0212] Test 1: Hardness test, conducted according to GB / T 2411-2008; density test, conducted according to GB / T6343-2009, determining the apparent core density. The compressibility and compressive modulus test methods are as follows:
[0213] A.1 Scope
[0214] This test method is applicable to determining the compressibility and compressive elasticity properties of polishing pads.
[0215] A.2 Test Equipment and Materials
[0216] Manual thickness gauge
[0217] A.3 State Adjustment
[0218] Before the test, the sample should be conditioned in a relaxed state for at least 2 hours and the test should be conducted at standard atmospheric pressure and 25±2℃.
[0219] A.4 Test Procedure
[0220] A.4.1 Cut five 30mm × 30mm samples from the polishing pad product and adjust them according to the conditions specified in A.3.
[0221] A.4.2 Clean the presser foot and lower the worktable, put down the presser foot, and zero the temperature (presser foot area is 0.785cm2).
[0222] A.4.3 Place the conditioned sample flat and tension-free on the worktable, add a 235.5g weight, hold the pressure for 30s, and record the light pressure thickness T0.
[0223] A.4.4 Add another 1177.5g weight, hold the pressure for 60s, and record the thickness of the pressure T1.
[0224] A.4.5 Immediately afterward, remove all weights, raise the pressure foot, and after the sample has recovered for 60 seconds, apply a 235.5g weight again. After maintaining the pressure for 30 seconds, measure the thickness under the second light pressure, i.e., the recovered thickness T2.
[0225] A.4 Result Processing
[0226] Compression ratio and compressive elasticity are calculated according to formulas A1 and A2:
[0227]
[0228]
[0229] In the formula:
[0230] C – Compression ratio, %
[0231] R – Compressive modulus, %
[0232] T0 – Lightly compressed load thickness, mm
[0233] T1 – Thickness under heavy load, mm
[0234] T2 – Secondary light load thickness, mm
[0235] Take the arithmetic mean of the five measurements.
[0236] Table 1 shows the results of static tests for hardness, density, compressibility, and compressive elasticity in the examples.
[0237]
[0238] Table 1-1 shows the results of static tests for hardness, density, compressibility, and compressive elasticity of the comparative examples.
[0239]
[0240] Test 2: Impact strength test was conducted in accordance with GB / T 1043.1-2008. The specimens were unnotched, with 10 specimens of each type. The impact direction of the simply supported beam was lateral. The results are shown in Table 2.
[0241] Table 2 shows the test results of performance test 2 in Example 2.
[0242]
[0243] Table 2-1 Performance Test Results of Comparative Example 2
[0244]
[0245] Test 3: Polishing performance test of polishing pad
[0246] Table 3 Polishing Test Parameters
[0247]
[0248] Table 4 shows the test results of Test 3 in Example 4.
[0249]
[0250]
[0251] Table 4-1 Test results of Comparative Example 3
[0252]
[0253]
[0254]
[0255] The performance test results above show that silica and diamond are in a fluid state in the system and are not solidified in the system. However, in the actual polishing process, both need to come into contact with the material being polished, and practical experience shows that a contact ratio of approximately 3:1 is optimal. How to achieve a balance between the two when they are immersed in the polyurethane porous material during preparation, and how to ensure that both can maintain stable performance under pressure during the later polishing process, is a great challenge. The inventors have found that by using two compounded organosilicon surfactants and having silica participate in the reaction in solution form, a polishing pad with superior performance can be obtained.
[0256] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.
Claims
1. A method for preparing a composite abrasive polishing pad containing a shear-thickening fluid, characterized in that, The steps are as follows: S01 Weigh out the polyurethane prepolymer, deionized water, polytetrahydrofuran diol, 3,3'-dichloro-4,4'-diphenylmethane diamine, triethylenediamine and polyol mixture and organosilicon surfactant according to the mass fractions. SO2 polyurethane prepolymer and polytetrahydrofuran diol were mixed at 80°C with high-speed stirring at 2000-2500 rpm to form material tank A. Deionized water, triethylenediamine and polyol mixture and organosilicon surfactant were mixed at room temperature at 2000 rpm to form material tank S. 3,3'-dichloro-4,4'-diphenylmethanediamine was kept at 120°C to form material tank C. Raw materials from S03 A, C, and S tanks are simultaneously mixed and discharged at a discharge port speed of 3500-4000 rpm. After discharge, the mixture is directly poured into a cylindrical mold with a diameter of 950 mm that is kept at 80℃. After all the mixed slurry has been poured into the mold, the mold cover is closed. The molding ratio is 1.
2. The sample is demolded after 2 hours at 80℃. S04 The sample block was placed in an oven and cured at 100℃ for 16 hours to obtain a cured sample block; S05 The sample block was sliced, and the thickness of the polyurethane microporous skeleton after slicing was 2.50mm±0.05mm; S06 The silica aqueous solution, single crystal diamond, deionized water, polycarboxylic acid anionic surfactant, and triethanolamine were weighed according to the mass fraction. The silica aqueous solution and single crystal diamond were mixed at high speed of 2000-2500rpm. Then, triethanolamine, polycarboxylic acid anionic surfactant, hydroxypropyl polydimethylsiloxane, and deionized water were added in sequence and stirred at 1500rpm to obtain a shear-thickened slurry; After the bottom of the S07 polyurethane microporous skeleton sheet is flatly laid with PET film, the shear thickening component is injected, the slurry is mixed in proportion, scraped flat, and left to stand at room temperature for 30 minutes to form. The polishing pad is composed of a polyurethane soft microporous framework, a shear-thickening fluid, and composite abrasives; wherein the density of the polyurethane soft microporous framework is 0.10-0.20 g / cm³. 3 The thickness is 2.50±0.5mm, and the average pore size is 200±50μm; the composite abrasive is made of silica aqueous solution and single crystal diamond.
2. The method of claim 1, wherein the polishing pad is prepared by the steps of: The silica in the aqueous silica solution has a particle size of 150-300 nm.
3. The method of claim 1, wherein the method further comprises the step of: The single-crystal diamond has a particle size of 500-1000 nm.
4. The method of claim 1 wherein the polishing pad is prepared by the steps of: The mass ratio of the silica aqueous solution to single-crystal diamond is 5:1 to 1:
5.
5. The method of claim 1 wherein the polishing pad is prepared by the steps of: The hardness of the polyurethane prepolymer is 73-75 Shore D.
6. The method of claim 1 wherein the polishing pad is prepared by the steps of: The silica aqueous solution is a silane-modified silica aqueous solution.
7. A composite abrasive polishing pad prepared by the method of any one of claims 1-6 containing a shear-thickening fluid, characterized in that, It is used in the field of SiC material processing.