CN116141214A - Preparation method of recyclable mixed abrasive polishing film - Google Patents

Preparation method of recyclable mixed abrasive polishing film Download PDF

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Publication number
CN116141214A
CN116141214A CN202210934985.XA CN202210934985A CN116141214A CN 116141214 A CN116141214 A CN 116141214A CN 202210934985 A CN202210934985 A CN 202210934985A CN 116141214 A CN116141214 A CN 116141214A
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abrasive
tpe
micron
sized
polishing
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CN202210934985.XA
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CN116141214B (en
Inventor
陆静
刘首麟
徐胜通
王嘉炜
柯聪明
罗求发
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Huaqiao University
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Huaqiao University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D11/00Constructional features of flexible abrasive materials; Special features in the manufacture of such materials
    • B24D11/001Manufacture of flexible abrasive materials
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/20Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
    • B24D3/28Resins or natural or synthetic macromolecular compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B24GRINDING; POLISHING
    • B24DTOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • B24D3/02Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent
    • B24D3/20Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents the constituent being used as bonding agent and being essentially organic
    • B24D3/28Resins or natural or synthetic macromolecular compounds
    • B24D3/32Resins or natural or synthetic macromolecular compounds for porous or cellular structure
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/62Plastics recycling; Rubber recycling

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Polishing Bodies And Polishing Tools (AREA)

Abstract

The invention discloses a preparation method of a recyclable mixed abrasive polishing film, which comprises the following steps: (1) Heating a thermoplastic elastomer (TPE) to a molten state to obtain a molten state TPE; (2) Uniformly mixing a micron-sized hard abrasive and a micron-sized rare earth abrasive to prepare a mixed abrasive; (3) uniformly mixing the mixed abrasive with the molten TPE; (4) Extruding and casting the material obtained in the step (3) to obtain the mixed abrasive polishing film. The mixed abrasive polishing film prepared by the invention has wide application range, is widely applicable to ceramic substrate polishing, flat stone surface polishing, semiconductor wafer polishing and precision machining of large-size planes, can be formed again by a simple extrusion casting method after being heated to a molten state under the condition of damage, and greatly reduces the preparation cost.

Description

Preparation method of recyclable mixed abrasive polishing film
Technical Field
The invention belongs to the technical field of ultra-precise machining tools, and particularly relates to a preparation method of a recyclable mixed abrasive polishing film.
Background
Currently in the field of ultra-precision machining, particularly polishing machining. Chemical mechanical polishing is used as the main stream method of polishing at present, different chemical reagents are added into polishing liquid, and the abrasive particles and the workpiece generate partial chemical reaction in the chemical reagent environment, so that the surface hardness of the workpiece is reduced, the quality of the processed surface can be improved, and the processing efficiency can also be improved. In terms of abrasive use, there are two types of free abrasive polishing and fixed abrasive polishing. Better surface quality can be obtained by polishing with a fixed abrasive, but the problems of scratch, serious damage to tools and the like can be caused. The free abrasive cannot control the track of the abrasive particles, so that the processing efficiency is low and the processing effect is poor. At present, a plurality of processing methods are to add high-hardness abrasive materials into a polishing film in a consolidation way, then to prepare slurry of micron-sized rare earth abrasive materials, and to prepare polishing liquid by mixing the slurry with various chemical reagents according to a proportion, so that the process is complicated and the storage is difficult. When the micron-sized rare earth abrasive is independently used as polishing abrasive, the processing effect is poor no matter the abrasive is added into a polishing film by using a consolidation method or is prepared into a free slurry form, and the requirements of no scratch and no surface defect on the surface processing of a wafer cannot be met at present. Meanwhile, after the polishing film of the fixed abrasive is used, the situation that the high polymer material and abrasive particles fall off can occur, so that the processing effect is poor, the service life is short, and the waste of resources is caused.
At present, domestic and foreign scholars develop polishing tools with different effects aiming at the problems, such as CN102825561A discloses a water-based polishing film and a preparation method thereof, CN104002252A discloses a superfine abrasive biopolymer flexible polishing film and a preparation method thereof, CN104275651A discloses a diamond polishing film preparation method and the like, and the defects of fixed abrasives are overcome to a certain extent, but the coating with abrasive particles is coated on the surface of a substrate in a smearing or electrostatic adsorption mode, so that a polishing workpiece can have certain abrasion on the polishing film after contacting with the polishing film, and the polishing film can be corroded and shed after the polishing solution with chemical reagent is added.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of a recyclable mixed abrasive polishing film.
The technical scheme of the invention is as follows:
a preparation method of a recyclable mixed abrasive polishing film comprises the following steps:
(1) Heating a thermoplastic elastomer (TPE) to a molten state to obtain a molten state TPE;
(2) Uniformly mixing a micron-sized hard abrasive and a micron-sized rare earth abrasive to prepare a mixed abrasive, wherein the particle size of the micron-sized hard abrasive is larger than that of the micron-sized rare earth abrasive;
(3) Uniformly mixing the mixed abrasive with the molten TPE according to the proportion of 20-40wt% to 60-80 wt%;
(4) Extruding and casting the material obtained in the step (3) to obtain the mixed abrasive polishing film.
In a preferred embodiment of the present invention, the thermoplastic elastomer TPE comprises at least one of styrenic TPE, olefinic TPE, diene TPE, vinyl chloride TPE and urethane TPE.
Further preferably, the thermoplastic elastomer TPE is a polyurethane TPE or an olefin TPE.
In a preferred embodiment of the present invention, the micron-sized hard abrasive is at least one of diamond, alumina, silicon carbide, and boron nitride.
Further preferably, the micron-sized hard abrasive is diamond or alumina.
Further preferably, the micron-sized hard abrasive has a particle size of W3-W20.
In a preferred embodiment of the present invention, the micron-sized rare earth abrasive is at least one of cerium oxide, yttrium oxide, lutetium oxide, and lanthanum oxide.
Further preferably, the micron-sized rare earth abrasive is cerium oxide and/or yttrium oxide.
Further preferably, the micron-sized rare earth abrasive has a particle size of W0.5-W2.
In a preferred embodiment of the present invention, the step (3) is: the mixed abrasive and the molten TPE are uniformly mixed according to the proportion of 25-40wt% to 60-75 wt%.
The beneficial effects of the invention are as follows:
1. the mixed abrasive polishing film prepared by the invention has wide application range and is widely suitable for polishing ceramic substrates, polishing flat stone surfaces, polishing semiconductor wafers and precisely machining large-size planes.
2. The invention adopts the processing method of the fixed abrasive, can effectively solve the problem that the processing of the free abrasive is uncontrollable, and ensures that the processing is more uniform.
3. The polishing film adopts a mode of mixing the high-hardness abrasive with the micron-sized rare earth abrasive, so that the fine-granularity micron-sized rare earth abrasive is better contacted with a workpiece to be processed in the polishing processing, and scratches and pit defects generated in the processing of the high-hardness abrasive can be eliminated in the CMP process.
4. According to the invention, the mixed abrasive is directly mixed with the thermoplastic elastomer TPE, and the thermoplastic elastomer TPE has the characteristics of good toughness, large damage tolerance and rebound resilience in the processing process, so that the damage of the high-hardness abrasive to the processing surface is reduced.
5. The thermoplastic elastomer TPE selected by the invention has the advantages of simple processing and molding, recycling and no environmental pollution, has higher mechanical energy, long service life, higher corrosion resistance and acid and alkali resistance, can be molded again by a simple extrusion casting method after being heated to a molten state under the condition of breakage, and greatly reduces the preparation cost.
6. The invention does not need long-time drying and cooling, and the large-size polishing film is directly manufactured by using an extrusion casting method, so that the prepared film has balanced performance and uniform thickness, can be cut according to the requirements for special shapes, and is suitable for mass production.
Drawings
FIG. 1 is a schematic view of an extrusion casting apparatus used in the examples of the present invention: no. 1 chill roll, no. 2 chill roll, shaping roller, peel off the roller, coiling mechanism, wherein shaping roller interval is 0.3mm.
FIG. 2 is a schematic representation of a cross-section of a mixed abrasive polishing film after formation in accordance with example 1 of the present invention.
FIG. 3 is a surface topography of a 2 inch GaN wafer processed by CMP with a mixed abrasive polishing film prepared in example 1 of the present invention.
FIG. 4 is a surface topography of a 2 inch GaN wafer processed by CMP after heat and melt reforming of a mixed abrasive polishing film prepared in example 1 of the present invention.
Fig. 5 is a surface topography of a 2 inch sapphire substrate CMP processed with a mixed abrasive polishing film prepared in example 2 of the present invention.
FIG. 6 is a surface topography of a 2 inch sapphire substrate processed by CMP after heat and melt reforming of a mixed abrasive polishing film prepared in example 2 of the present invention.
FIG. 7 is a surface topography of a conventional consolidated polishing film prepared in comparative example 1 of the present invention with free abrasive grains added to CMP process 2 inch gallium nitride.
Detailed Description
The technical scheme of the invention is further illustrated and described below by the specific embodiments in combination with the accompanying drawings.
Example 1
Selecting polyurethane TPE (TPU 9392A), and heating to 200 ℃ to enable the TPE to be in a molten state; the W5 alumina is selected as a high-hardness abrasive, and the high-hardness abrasive, the W0.5 cerium oxide and the W0.5 yttrium oxide are mixed according to the mass ratio of 1:2:2 to prepare the mixed abrasive. The molten TPU and the mixed abrasive are uniformly mixed according to the weight percentage of 60 to 40. Pouring the mixed solvent into extrusion casting film equipment directly. The extrusion casting apparatus is shown in fig. 1. After processing, the large-size polishing film roll can be directly prepared, and the mixed abrasive polishing film is prepared. The cross section of the formed mixed abrasive polishing film is shown in fig. 2. The mixed abrasive polishing film is cut and then stuck to a UNIPO-1200S automatic grinding polisher, the rotation speed of a carrying disc is 60rpm, the rotation speed of a polishing disc is 120rpm, the polishing pressure is set to be 0.5kg, 4% potassium persulfate is selected as polishing liquid, a 2-inch gallium nitride wafer with the original roughness surface of 10nm is polished for 1h, the surface roughness can reach 0.40nm, and no obvious scratches and pits exist on the surface of the wafer. The results are shown in FIG. 3. After the cumulative processing for 6 hours, the polishing film appeared slightly dented at the processing place of the wafer. After heating, melting and extrusion molding, the 2-inch gallium nitride wafer with the original roughness surface of 10nm is polished for 1h again, the surface roughness can reach 0.38nm, and no obvious scratches and pits are formed on the surface of the wafer. The results are shown in FIG. 4.
Example 2
An olefin TPE (TPO 185) is selected and heated to 220 ℃ to be in a molten state; the W10 diamond is selected as a high-hardness abrasive and is mixed with rare earth abrasive W1 cerium oxide according to the mass ratio of 1:8 to prepare the mixed abrasive. The molten TPO and the mixed abrasive are uniformly mixed according to the weight percentage of 75 to 25. Pouring the mixed solvent into extrusion casting film equipment directly. The extrusion casting apparatus is shown in fig. 1. After processing, the large-size polishing film roll can be directly prepared, and the mixed abrasive polishing film is prepared. The cross section of the formed mixed abrasive polishing film is shown in fig. 2. The mixed abrasive polishing film is cut and then stuck to a UNIPO-1200S automatic grinding polisher, the rotation speed of a carrying disc is 65rpm, the rotation speed of a polishing disc is 130rpm, the polishing pressure is set to be 0.4kg, 2% hydrogen peroxide is selected as polishing liquid, the 2 inch sapphire substrate with the original roughness surface of 15nm is polished for 1h, the surface roughness can reach 0.42nm, and no obvious scratches and pits exist on the surface of a wafer. The results are shown in FIG. 5. After 5 hours of cumulative processing, the polishing film appeared slightly dented at the processing site of the wafer. After heating, melting and extrusion molding, the 2-inch sapphire substrate with the original roughness surface of 15nm is polished for 1h again, the surface roughness can reach 0.36nm, and no obvious scratches and pits are formed on the surface of the wafer. The results are shown in FIG. 6.
Comparative example 1
A common consolidated form of the polishing film was selected, the abrasive particles selected for W5 alumina, and the abrasive concentration was 20wt%. Meanwhile, 10wt percent of W0.5 cerium oxide, 10wt percent of W0.5 yttrium oxide and 4 percent of potassium persulfate are taken to prepare rare earth abrasive slurry. And the polishing pressure is set to be 0.5kg, and the 2-inch gallium nitride wafer with the original roughness surface of 10nm is polished for 1h, wherein the surface roughness can only reach 1nm, but slight scratches exist, and the ultra-smooth surface without scratches and surface defects cannot be achieved. The results are shown in FIG. 7. And the situation that the abrasive particles on the polishing film fall off occurs after the accumulated processing is carried out for 1.5 hours. If the processing is to be continued, a new polishing film needs to be replaced.
The foregoing description is only illustrative of the preferred embodiments of the present invention and is not to be construed as limiting the scope of the invention, i.e., the invention is not to be limited to the details of the invention.

Claims (10)

1. A preparation method of a recyclable mixed abrasive polishing film is characterized by comprising the following steps: the method comprises the following steps:
(1) Heating a thermoplastic elastomer (TPE) to a molten state to obtain a molten state TPE;
(2) Uniformly mixing a micron-sized hard abrasive and a micron-sized rare earth abrasive to prepare a mixed abrasive, wherein the particle size of the micron-sized hard abrasive is larger than that of the micron-sized rare earth abrasive;
(3) Mixing the abrasive with the molten TPE in an amount of 20 to 40wt%: mixing evenly in a proportion of 60-80 wt%;
(4) Extruding and casting the material obtained in the step (3) to obtain the mixed abrasive polishing film.
2. The method of manufacturing according to claim 1, wherein: the thermoplastic elastomer TPE includes at least one of a styrenic TPE, an olefinic TPE, a diene TPE, a vinyl chloride TPE, and a urethane TPE.
3. The method of manufacturing as claimed in claim 2, wherein: the thermoplastic elastomer TPE is polyurethane TPE or olefin TPE.
4. The method of manufacturing according to claim 1, wherein: the micron-sized hard abrasive is at least one of diamond, alumina, silicon carbide and boron nitride.
5. The method of manufacturing according to claim 4, wherein: the micron-sized hard abrasive is diamond or aluminum oxide.
6. The method of claim 4 or 5, wherein: the granularity of the micron-sized hard abrasive is W3-W20.
7. The method of manufacturing according to claim 1, wherein: the micron-sized rare earth abrasive is at least one of cerium oxide, yttrium oxide, lutetium oxide and lanthanum oxide.
8. The method of manufacturing according to claim 7, wherein: the micron-sized rare earth abrasive is cerium oxide and/or yttrium oxide.
9. The method of claim 7 or 8, wherein: the granularity of the micron-sized rare earth abrasive is W0.5-W2.
10. The method of preparing as claimed in claim 9, wherein: the step (3) is as follows: mixing the abrasive with the molten TPE in an amount of 25 to 40wt%: mixing evenly in the proportion of 60-75wt%.
CN202210934985.XA 2022-08-04 2022-08-04 Preparation method of recyclable mixed abrasive polishing film Active CN116141214B (en)

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004311727A (en) * 2003-04-07 2004-11-04 Hitachi Chem Co Ltd Polishing pad, its manufacturing method and polishing method using it
CN1669739A (en) * 2000-12-01 2005-09-21 东洋橡膠工业株式会社 Polishing pad, method of manufacturing the polishing pad, and cushion layer for polishing pad
US20060199473A1 (en) * 2003-04-03 2006-09-07 Masao Suzuki Polishing pad, process for producing the same and method of polishing therewith
CN101208178A (en) * 2005-06-30 2008-06-25 卡伯特微电子公司 Use of CMP for aluminum mirror and solar cell fabrication
JP2008207324A (en) * 2007-02-01 2008-09-11 Kuraray Co Ltd Polishing pad and manufacturing method for the polishing pad
JP2009078332A (en) * 2007-09-27 2009-04-16 Kuraray Co Ltd Fiber composite polishing pad
CN108472788A (en) * 2015-12-30 2018-08-31 圣戈班磨料磨具有限公司 Milling tool and its forming method
CN111918992A (en) * 2018-03-27 2020-11-10 哈伯西有限公司 Abrasive product comprising impregnated woven fabric and abrasive particles

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1669739A (en) * 2000-12-01 2005-09-21 东洋橡膠工业株式会社 Polishing pad, method of manufacturing the polishing pad, and cushion layer for polishing pad
US20060199473A1 (en) * 2003-04-03 2006-09-07 Masao Suzuki Polishing pad, process for producing the same and method of polishing therewith
JP2004311727A (en) * 2003-04-07 2004-11-04 Hitachi Chem Co Ltd Polishing pad, its manufacturing method and polishing method using it
CN101208178A (en) * 2005-06-30 2008-06-25 卡伯特微电子公司 Use of CMP for aluminum mirror and solar cell fabrication
JP2008207324A (en) * 2007-02-01 2008-09-11 Kuraray Co Ltd Polishing pad and manufacturing method for the polishing pad
JP2009078332A (en) * 2007-09-27 2009-04-16 Kuraray Co Ltd Fiber composite polishing pad
CN108472788A (en) * 2015-12-30 2018-08-31 圣戈班磨料磨具有限公司 Milling tool and its forming method
CN111918992A (en) * 2018-03-27 2020-11-10 哈伯西有限公司 Abrasive product comprising impregnated woven fabric and abrasive particles

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