CN114536212A - Microporous thermoplastic polyurethane polishing pad and semi-continuous preparation method thereof - Google Patents
Microporous thermoplastic polyurethane polishing pad and semi-continuous preparation method thereof Download PDFInfo
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- CN114536212A CN114536212A CN202210110517.0A CN202210110517A CN114536212A CN 114536212 A CN114536212 A CN 114536212A CN 202210110517 A CN202210110517 A CN 202210110517A CN 114536212 A CN114536212 A CN 114536212A
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- 229920002803 thermoplastic polyurethane Polymers 0.000 title claims abstract description 101
- 238000005498 polishing Methods 0.000 title claims abstract description 83
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 45
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000012530 fluid Substances 0.000 claims abstract description 35
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000005187 foaming Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 21
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 20
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- 238000005096 rolling process Methods 0.000 claims abstract description 11
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 7
- 238000005470 impregnation Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 238000004080 punching Methods 0.000 claims abstract description 4
- 239000002243 precursor Substances 0.000 claims description 15
- 238000011437 continuous method Methods 0.000 claims description 14
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- 239000003963 antioxidant agent Substances 0.000 claims description 5
- 230000003078 antioxidant effect Effects 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 5
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- 238000001125 extrusion Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 4
- 238000003490 calendering Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010924 continuous production Methods 0.000 claims 1
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- 230000000694 effects Effects 0.000 abstract description 9
- 239000006260 foam Substances 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/11—Lapping tools
- B24B37/20—Lapping pads for working plane surfaces
- B24B37/24—Lapping pads for working plane surfaces characterised by the composition or properties of the pad materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D18/00—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for
-
- 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
- B24D18/0027—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for by impregnation
-
- 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
- B24D18/0072—Manufacture of grinding tools or other grinding devices, e.g. wheels, not otherwise provided for using adhesives for bonding abrasive particles or grinding elements to a support, e.g. by gluing
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/122—Hydrogen, oxygen, CO2, nitrogen or noble gases
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/06—CO2, N2 or noble gases
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
- Mechanical Treatment Of Semiconductor (AREA)
Abstract
The invention discloses a microporous thermoplastic polyurethane polishing pad and a semi-continuous preparation method thereof, and relates to the technical field of integrated circuit materials. The semi-continuous preparation method of the microporous thermoplastic polyurethane polishing pad comprises the following steps: (1) melting, extruding, rolling and rolling the high-hardness thermoplastic polyurethane and the auxiliary agent; (2) carrying out high-pressure fluid impregnation, low-temperature air locking, low-temperature storage, heating foaming and rolling on the coiled material to obtain a foamed coiled material; (3) peeling and punching the foaming coiled material to obtain an upper-layer cushion; (4) grinding, slotting and attaching the upper cushion or the cushion layer and the gumObtaining a microporous thermoplastic polyurethane polishing pad; the hardness of the high-hardness thermoplastic polyurethane is 55-85 HD; the upper layer pad has a hardness of 25 to 80HD, a thickness of 1.3 to 2.0mm and a density of 0.1 to 1.0g/cm3The size of the foam hole is 1-200 μm; the high-pressure fluid is carbon dioxide and nitrogen. The polishing pad prepared by the method of the present invention has excellent polishing effect and polishing rate.
Description
Technical Field
The invention relates to the technical field of integrated circuit materials, in particular to a microporous thermoplastic polyurethane polishing pad and a semi-continuous preparation method thereof.
Background
Chemical-mechanical polishing (CMP) processes are used for surface planarization of semiconductor devices, gemstones, glass, and the like. Planarization is required, for example, in the manufacture of semiconductor devices by forming various process layers on a wafer, selectively removing or patterning portions of such layers, and depositing further process layers on the wafer. The CMP polishing process requires a polishing pad and a polishing liquid. In a typical CMP process, a wafer guide is mounted on a carrier in a CMP tool, a force is applied to the carrier and the wafer against a polishing pad, the carrier and the wafer are rotated on a CMP tool polishing table, a polishing liquid is introduced between the wafer and the polishing pad during polishing, and portions of the layer of polishing material are removed under chemical and mechanical forces. Since the process layer may comprise an insulating layer, a gate oxide layer, a conductive layer, a metal or glass layer, etc., the polishing pad and the polishing solution need to be coordinated to uniformly remove different materials within the layer, the same or similar removal rates result in a planarized process layer, and the different removal rates result in defects in the process layer. As integrated circuit feature sizes decrease, CMP-induced defects are magnified.
Porous polyurethanes have proven to be a class of materials that produce high performance polishing pads with consistently reproducible polishing characteristics. The prior art of porous polyurethane materials is to pour a polyurethane foam stock solution into a porous cake and cut the porous cake into polishing pads of several thicknesses. The polyurethane foaming stock solution generates a large amount of heat in the foaming process, and the foaming structure is insulated to hinder the dissipation of the heat, so that a macroporous structure and wide pore size distribution of a porous polyurethane core layer are caused, and the performance consistency of the microporous polyurethane polishing pad is influenced; meanwhile, the pouring mold is of a disc structure, the processing mode is intermittent and inefficient, and continuous porous polyurethane sheets are difficult to prepare. Therefore, it is desirable to provide a method for preparing a porous polyurethane sheet with simple processing and good processing effect.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a microporous thermoplastic polyurethane polishing pad and a semi-continuous preparation method thereof, the method can be used for efficiently producing the polishing pad, and the prepared polishing pad has good polishing efficiency and polishing effect.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a semi-continuous method of making a microporous thermoplastic polyurethane polishing pad, the method comprising:
(1) drying, premixing, continuously extruding by a double screw rod, rolling and rolling the high-hardness thermoplastic polyurethane and the auxiliary agent to obtain a precursor high-hardness thermoplastic polyurethane coiled material;
(2) dipping the precursor high-hardness thermoplastic polyurethane coiled material by high-pressure fluid, locking gas at low temperature, storing at low temperature, heating for foaming, and continuously rolling to obtain the high-hardness thermoplastic polyurethane foaming coiled material;
(3) peeling and continuously punching the high-hardness thermoplastic polyurethane foaming coiled material to obtain an upper-layer cushion;
(4) grinding and grooving the upper-layer pad, and attaching the back glue or attaching the buffer layer and the back glue to obtain the microporous thermoplastic polyurethane polishing pad;
the hardness of the high-hardness thermoplastic polyurethane is 55-85 HD; the upper layer pad has a hardness of 25 to 80HD, a thickness of 1.3 to 2.0mm and a density of 0.1 to 1.0g/cm3The average cell size is 1-200 μm;
the high-pressure fluid is carbon dioxide and nitrogen.
According to the invention, the thermoplastic polyurethane with the hardness of 55-90 HD is selected to prepare the polishing pad, so that the polishing pad has enough hardness to remove an oxide layer and the like on the surface of a wafer, and has certain removal efficiency; by selecting two high-pressure fluids of carbon dioxide and nitrogen to dip the precursor high-hardness thermoplastic polyurethane, the upper-layer pad can be smoother, the cell structure is more uniform, and the polishing pad has a good polishing effect and generates few scratches on the surface of a polished object.
Preferably, in the step (2), the impregnation process is performed in two steps, wherein a carbon dioxide fluid of 2-10 MPa is injected first, and then a nitrogen fluid of 0.1-5 MPa is injected.
The carbon dioxide fluid can diffuse fast in the thermoplastic polyurethane coiled material, has high solubility and is beneficial to preparing the low-density thermoplastic polyurethane foaming coiled material, but the carbon dioxide fluid has high desorption speed in the foaming process of the thermoplastic polyurethane coiled material, so that the phenomena of large holes on the surface of the thermoplastic polyurethane foaming coiled material, uneven cell sizes, obvious volume shrinkage and surface wrinkle of a product are easily caused. The nitrogen fluid has relatively low solubility in the thermoplastic polyurethane web, low diffusion coefficient, and is easy to increase the density of the thermoplastic polyurethane foamed web, but has excellent surface quality. The inventor of the application proves through a large number of experiments that the thermoplastic polyurethane coiled material is impregnated by using the carbon dioxide fluid and the nitrogen fluid in sequence, so that the thermoplastic polyurethane foamed coiled material with low density, high surface evenness and uniform cell structure can be prepared, and the polishing pad prepared from the foamed coiled material has good polishing efficiency and polishing effect.
Further preferably, in the dipping process, a carbon dioxide fluid with the pressure of 3-8 MPa is injected firstly, and then a nitrogen fluid with the pressure of 0.5-4 MPa is injected. Controlling the pressure of both within the above range can further improve the overall performance of the polishing pad.
Preferably, in the step (2), the mass content of the high-pressure fluid in the impregnated thermoplastic polyurethane coiled material obtained after impregnation is 1-10%.
The content (%) of the high-pressure fluid in the high-hardness thermoplastic polyurethane coiled material is equal to (m)1-m0)×100％/m0(ii) a Wherein m is0Mass m of precursor high-hardness thermoplastic polyurethane coil1The quality of the dipped high-hardness thermoplastic polyurethane coiled material is that after high-pressure fluid dipping and normal-temperature and normal-pressure desorption for 10 min. By optimizing the impregnation content of the high pressure fluid, the density, cell size, cell density, etc. of the subsequent product can be further controlled.
Preferably, in the step (1), the extrusion temperature is: 190-220 ℃ and the temperature of the extruder die head is 210-220 ℃; and cooling the calendering roller by adopting cooling water at 5-15 ℃.
Preferably, in the step (2), the air is locked at a low temperature of-18-0 ℃, then the product is stored at a low temperature of-18-15 ℃, and then a heating medium is introduced for physical foaming. The high-hardness thermoplastic polyurethane of the present invention has a vitrification phenomenon at-20 to-50 deg.c, and thus can restrict the escape of the movement of high-pressure fluid while the temperature is maintained within the above-mentioned preferred range.
Preferably, the thickness of the precursor high-hardness thermoplastic polyurethane coiled material is 1-3 mm; the high-hardness thermoplastic polyurethane foaming coiled material has the thickness of 2-5 mm and the density of 0.1-1.0 g/cm3The average cell size is 1 to 200 μm, and the hardness is 20 to 80 HD. For the high-hardness thermoplastic polyurethane disclosed by the invention, the extrusion processing process is difficult, a coiled material with a very high thickness is difficult to prepare, the flatness of the coiled material with the thickness of more than 3mm is relatively poor, and when the thickness of the precursor high-hardness thermoplastic polyurethane coiled material is less than 1mm, the later foaming effect is poor.
Preferably, when the thickness of the high-hardness thermoplastic polyurethane foaming coiled material is 2-3 mm, continuously sectioning and peeling to obtain an upper cushion with a uniform cell structure on one side and a non-foaming skin layer structure on the other side; when the thickness of the high-hardness thermoplastic polyurethane foaming coiled material is 3.1-4 mm, continuously cutting and peeling to obtain an upper-layer cushion with uniform cell structures on two surfaces; and (4) when the thickness of the high-hardness thermoplastic polyurethane coiled material obtained in the step (3) is 4.1-5.0mm, continuously cutting, peeling and cutting to obtain two rolls of upper-layer mats with uniform cell structures on single surfaces.
Preferably, the auxiliary agent is an antioxidant and a lubricant, and the auxiliary agent accounts for 0.5-5% of the high-hardness thermoplastic polyurethane by mass. The antioxidant is added to improve the stability of the product, the lubricant is added to improve the processing performance of the thermoplastic polyurethane, and the components of the prepared product are more uniform.
Meanwhile, the invention also discloses the microporous thermoplastic polyurethane polishing pad prepared by the method.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the preparation raw materials of the upper pad in the polishing pad are selected, and the high-pressure fluid is controlled to be the carbon dioxide fluid and the nitrogen fluid, so that the preparation method of the polishing pad is simplified, the method can realize semi-continuous processing, the processing efficiency is high, the processing cost is low, and the prepared polishing pad has good polishing effect and polishing efficiency. The microporous thermoplastic polyurethane polishing pad can be applied to the field of polishing of semiconductor wafers, jewels and glass.
Drawings
FIG. 1 is a schematic diagram of the continuous die cutting process for making microporous thermoplastic polyurethane polishing pads according to the present invention;
FIG. 2 is an optical view of a high hardness thermoplastic polyurethane foamed web of the present invention;
FIG. 3 is an optical diagram of the upper pad of the present invention.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
The materials used in the examples and comparative examples are as follows:
high-hardness thermoplastic polyurethane 1: lublorun ESTANE 58133 with a hardness of 55 HD;
high hardness thermoplastic polyurethane 2: lublorun ESTANE 58144 with a hardness of 65 HD;
high-hardness thermoplastic polyurethane 3: lublorun ESTANE ETE 75DT3 with hardness of 75 HD;
high hardness thermoplastic polyurethane 4: lobomoisten Isoplast 101LGF60 ETP with a hardness of 89D
Buffer layer: is sold on the market;
back gluing: is sold on the market;
lubricant: stearic acid, commercially available;
antioxidant: antioxidant 1010, commercially available.
Example 1
In one embodiment of the present invention, a method for semi-continuously preparing a microporous thermoplastic polyurethane polishing pad comprises the following steps:
(1) sequentially drying, premixing, continuously extruding by using a double screw rod, calendering and rolling 100 parts of high-hardness thermoplastic polyurethane 1 and 2 parts of lubricant and 0.5 part of antioxidant to obtain a precursor high-hardness thermoplastic polyurethane coiled material, wherein the temperature of an extruder from a feeding port to a fourth temperature zone is sequentially set to 199 ℃, 204 ℃, 210 ℃, 215 ℃ and 216 ℃, the temperature of a calender is controlled by using 10 ℃ circulating water, the temperature of an extruder die head is 213 +/-0.2 ℃, and the temperature is controlled by using heat conducting oil independently;
(2) injecting 5MPa carbon dioxide into the precursor thermoplastic polyurethane coiled material, then injecting 3MPa nitrogen to achieve dissolution balance, then locking gas at 0 ℃, storing at low temperature of 0 ℃ for 6h, heating and foaming by using hot air, and continuously rolling to obtain the high-hardness thermoplastic polyurethane foaming coiled material;
(3) continuously cutting the high-hardness thermoplastic polyurethane foaming coiled material, peeling one side of the high-hardness thermoplastic polyurethane foaming coiled material, and continuously punching to obtain a microporous thermoplastic polyurethane upper-layer pad;
(4) and (3) grinding the upper-layer pad, grooving (the groove is in a spiral line shape), and attaching the buffer layer and the gum to obtain the microporous thermoplastic polyurethane polishing pad.
Examples 2 to 3
In the embodiments of the semi-continuous preparation method of the microporous thermoplastic polyurethane polishing pad of the present invention, the difference between the embodiments 2 to 3 and the embodiment 1 is only that the types of the high hardness thermoplastic polyurethane used are different, and the high hardness thermoplastic polyurethane is 2 to 3.
Example 4
One embodiment of the semi-continuous method of making a microporous thermoplastic polyurethane polishing pad of the present invention differs from embodiment 1 only in that in step (2), 3MPa of carbon dioxide is injected into the precursor thermoplastic polyurethane web, followed by 4MPa of nitrogen fluid.
Example 5
One embodiment of the semi-continuous method of making a microporous thermoplastic polyurethane polishing pad of the present invention differs from embodiment 1 only in that in step (2), 8MPa of carbon dioxide is injected into the precursor thermoplastic polyurethane web, followed by 0.5MPa of nitrogen fluid.
Example 6
One embodiment of the semi-continuous method of making a microporous thermoplastic polyurethane polishing pad of the present invention differs from embodiment 1 only in that in step (2), 2MPa of carbon dioxide is injected into the precursor thermoplastic polyurethane web, followed by 5MPa of nitrogen.
Example 7
In one embodiment of the semi-continuous method for producing a microporous thermoplastic polyurethane polishing pad of the present invention, this embodiment differs from embodiment 1 only in that in step (2), 10MPa of carbon dioxide is injected into the precursor thermoplastic polyurethane web, followed by 0.1MPa of nitrogen.
Example 8
One example of a semi-continuous method of making a microporous thermoplastic polyurethane polishing pad of the present invention differs from example 1 only in that double-sided peeling is performed.
Example 9
An example of a semi-continuous method of making a microporous thermoplastic polyurethane polishing pad of the present invention differs from example 1 only in that there is no buffer layer in the polishing pad.
Comparative example 1
A method of making a microporous thermoplastic polyurethane polishing pad that differed from example 1 only in that only carbon dioxide was used during the high pressure fluid impregnation, at a pressure of 10 MPa.
Comparative example 2
A method of making a microporous thermoplastic polyurethane polishing pad that differed from example 1 only in that the thermoplastic polyurethane used in making the upper pad was high hardness thermoplastic polyurethane 4.
The intermediate products and the final products of examples and comparative examples were subjected to a performance test in which the polishing efficiency and polishing effect of the polishing pad were measured after the polishing pad polished copper in a 12-inch wafer; the test results are shown in table 1.
TABLE 1
As can be seen from the above test results, the polishing pads of examples 1-9 all had good polishing rates and polishing effects, and the polishing rates were all within the range
Min @93rpm, more than 2.0psi, and within 5 defects, and can meet the requirements of most enterprises. In comparative example 1, since the high-pressure fluid used was carbon dioxide, the density of the upper pad prepared was extremely low, wrinkles and large pores appeared on the surface of the foamed web, and the polishing efficiency of the polishing pad was seriously affected; the high-hardness thermoplastic polyurethane selected in comparative example 2 had too high hardness, resulting in difficulty in extrusion, and the extruded thermoplastic polyurethane sheet had a thickness of less than 0.5mm and unstable foaming, and could not be used to prepare a polishing pad.
In addition, it can be seen from the above test results that the pressure of the carbon dioxide fluid in example 6 is too low, which results in a low mass content of the high pressure fluid and a high density of the upper pad, which results in a high probability of generating defects during the polishing process, and the number of defects is relatively high, whereas in example 7, which is just the opposite, the density of the upper pad is low and the polishing rate is low.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A semi-continuous method for preparing a microporous thermoplastic polyurethane polishing pad, the method comprising:
(1) drying, premixing, continuously extruding by a double screw rod, rolling and rolling the high-hardness thermoplastic polyurethane and the auxiliary agent to obtain a precursor high-hardness thermoplastic polyurethane coiled material;
(2) dipping the precursor high-hardness thermoplastic polyurethane coiled material by high-pressure fluid, locking gas at low temperature, storing at low temperature, heating for foaming, and continuously rolling to obtain the high-hardness thermoplastic polyurethane foaming coiled material;
(3) peeling and punching the high-hardness thermoplastic polyurethane foaming coiled material to obtain an upper-layer cushion;
(4) grinding and grooving the upper-layer pad, and attaching the back glue or attaching the buffer layer and the back glue to obtain the microporous thermoplastic polyurethane polishing pad;
the hardness of the high-hardness thermoplastic polyurethane is 55-85 HD; the upper layer pad has a hardness of 25 to 80HD, a thickness of 1.3 to 2.0mm, and a density of 0.1 to 1.0g/cm3The average cell size is 1-200 μm;
the high-pressure fluid is carbon dioxide and nitrogen.
2. The semi-continuous method of preparing a microporous thermoplastic polyurethane polishing pad according to claim 1, wherein in step (2), the impregnation is performed in two steps, first injecting a carbon dioxide fluid at 2 to 10MPa, and then injecting a nitrogen fluid at 0.1 to 5 MPa.
3. The semi-continuous method of making a microporous thermoplastic polyurethane polishing pad of claim 2, wherein during the dipping step, the carbon dioxide fluid is injected at 3 to 8MPa, followed by the nitrogen fluid at 0.5 to 4 MPa.
4. The semi-continuous method of making a microporous thermoplastic polyurethane polishing pad of claim 1, wherein in step (2), the impregnated thermoplastic polyurethane web after impregnation has a high pressure fluid content of 1 to 10% by mass.
5. The semi-continuous method of making a microporous thermoplastic polyurethane polishing pad of claim 1, wherein in step (1), the extrusion temperature is: 190-220 ℃ and the temperature of the extruder die head is 210-220 ℃; and cooling the calendering roller by adopting a cooling medium at 5-15 ℃.
6. The semi-continuous process for preparing a microporous thermoplastic polyurethane polishing pad according to claim 1, wherein in step (2), the gas is locked at a low temperature of-18 to 0 ℃, then stored at a low temperature of-18 to 15 ℃, and then physically foamed by introducing a heating medium.
7. The semi-continuous method of making a microporous thermoplastic polyurethane polishing pad of claim 1, wherein the precursor high hardness thermoplastic polyurethane web has a thickness of 1 to 3 mm; the high-hardness thermoplastic polyurethane foaming coiled material has the thickness of 2-5 mm and the density of 0.1-1.0 g/cm3The average cell size is 1 to 200 μm, and the hardness is 20 to 75 HD.
8. The semi-continuous preparation method of a microporous thermoplastic polyurethane polishing pad according to claim 7, wherein when the thickness of the high-hardness thermoplastic polyurethane foamed coiled material is 2-3 mm, the upper pad with a uniform cell structure on one side and a non-foamed skin layer structure on the other side is obtained by continuously cutting and peeling; when the thickness of the high-hardness thermoplastic polyurethane foaming coiled material is 3.1-4 mm, continuously cutting and peeling to obtain an upper layer cushion with uniform cell structures on two surfaces; and (4) when the thickness of the high-hardness thermoplastic polyurethane coiled material obtained in the step (3) is 4.1-5.0mm, continuously cutting, peeling and cutting to obtain two rolls of upper-layer mats with uniform cell structures on single surfaces.
9. The semi-continuous method of making a microporous thermoplastic polyurethane polishing pad of claim 1, wherein the auxiliary agent is an antioxidant and a lubricant, the auxiliary agent comprising 0.5 to 5% by weight of the high hardness thermoplastic polyurethane.
10. A microporous thermoplastic polyurethane polishing pad prepared by the method of any one of claims 1 to 9.
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