WO2016006476A1 - 研磨フィルム - Google Patents
研磨フィルム Download PDFInfo
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- WO2016006476A1 WO2016006476A1 PCT/JP2015/068488 JP2015068488W WO2016006476A1 WO 2016006476 A1 WO2016006476 A1 WO 2016006476A1 JP 2015068488 W JP2015068488 W JP 2015068488W WO 2016006476 A1 WO2016006476 A1 WO 2016006476A1
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- WIPO (PCT)
- Prior art keywords
- polishing
- mass
- abrasive particles
- polishing layer
- film
- Prior art date
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D11/00—Constructional features of flexible abrasive materials; Special features in the manufacture of such materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
- B24D3/02—Physical 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
- B24D3/20—Physical 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
- B24D3/28—Resins or natural or synthetic macromolecular compounds
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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
- B24B19/00—Single-purpose machines or devices for particular grinding operations not covered by any other main group
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/11—Lapping tools
- B24B37/20—Lapping pads for working plane surfaces
- B24B37/24—Lapping pads for working plane surfaces characterised by the composition or properties of the pad materials
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
- B24D11/00—Constructional features of flexible abrasive materials; Special features in the manufacture of such materials
- B24D11/001—Manufacture of flexible abrasive materials
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/24—Coupling light guides
- G02B6/25—Preparing the ends of light guides for coupling, e.g. cutting
Definitions
- the present invention relates to an abrasive film.
- optical connectors that are easy to remove are widely used for connecting optical fibers. This connection is made by directly matching a ferrule that aligns optical fibers. For this reason, in order to reduce the optical loss (communication loss) of the optical fiber after connection, the connection end surface of the optical fiber connector to be connected is sufficiently smooth and a gap is formed between the optical fibers at the connection end surface. It is required that no optical fiber is drawn into the ferrule.
- Polishing of the connection end face of such an optical fiber connector is performed by four processes of an adhesive removing process, a rough spherical polishing process, an intermediate finishing process, and a final polishing process. Among them, the polishing accuracy of the final polishing process is large in light loss. Affect. Furthermore, from the viewpoint of productivity and production cost, a high grinding force is required for the polishing film used in the finish polishing step.
- an abrasive film provided with an abrasive layer having a resin binder and abrasive particles has been proposed.
- the type of resin binder and abrasive particles are selected, and the abrasive particle diameter is increased. (See JP-A-8-336758, JP-A-2002-239924, and JP-A-2007-190613).
- the optical fiber is selectively polished, and the optical fiber protrudes from the ferrule while preventing the optical fiber from being drawn. It is difficult to do so, and a gap is easily generated between the optical fibers at the connection end face. For this reason, in the said prior art, coexistence with high grinding force and the drawing-in prevention of an optical fiber is not enough.
- the present invention has been made in view of these circumstances, and an object thereof is to provide a polishing film that has a high grinding force and can prevent drawing of an optical fiber after polishing.
- the present inventors have found that the pulling of the optical fiber can be prevented by controlling the indentation hardness of the polishing layer and the content of abrasive particles having a large primary particle diameter.
- the inventors of the present invention have found that an abrasive film capable of preventing the optical fiber from being pulled in while using abrasive particles having a large primary particle diameter has been obtained, thereby completing the present invention.
- the invention made to solve the above problems is a polishing film having a base material and a polishing layer laminated on the surface thereof, wherein the polishing layer is dispersed in the resin binder and the resin binder.
- the content of abrasive particles having a primary particle diameter of 70 nm or more with respect to the entire abrasive particles is 10% by mass or more and 50% by mass or less, and the content of the abrasive particles in the polishing layer is 84% by mass.
- the indentation hardness of the polishing layer is 370 N / mm 2 or less.
- the indentation hardness of the polishing layer is less than or equal to the above upper limit, and the content of abrasive particles having a primary particle diameter of 70 nm or more with respect to the entire abrasive particles is less than or equal to the upper limit, thereby preventing the optical fiber from being pulled after polishing. it can.
- the content of abrasive particles having a primary particle diameter of 70 nm or more with respect to the entire abrasive particles is equal to or higher than the lower limit and the content of the abrasive particles in the polishing layer is equal to or higher than the lower limit, the abrasive film has a high grinding force.
- the abrasive particles are preferably silica particles.
- Silica particles are suitable for the final finishing process where a small surface roughness is required on the connection end face of the optical fiber connector. By using silica particles with a large primary particle size, higher grinding is achieved while maintaining polishing accuracy. Power can be given.
- the average thickness of the polishing layer is preferably 4 ⁇ m or more and 15 ⁇ m or less.
- the indentation hardness of the polishing layer can be kept low, the optical fiber can be more easily prevented from being pulled in, and the wear resistance of the polishing layer can be enhanced. .
- the resin binder preferably contains an elastomer having a glass transition temperature of 20 ° C. or less, and the content of the elastomer relative to the resin binder is preferably 20% by mass or more.
- polishing layer can be easily controlled by making the elastomer of the glass transition temperature 20 degrees C or less which the said resin binder contains into the said minimum or more.
- indentation hardness means a value measured in accordance with ISO-14477-1.
- primary particles refer to particles that are considered to be unit particles as judged from the apparent geometric form
- primary particle diameter refers to a scanning electron microscope (SEM) or a transmission electron microscope (TEM). ) Means the diameter of a single particle measured using the image of the particle observed using “”, and “particle diameter” refers to the diameter of the smallest circle circumscribing the image of this particle.
- the polishing film of the present invention can prevent the drawing of the optical fiber after polishing while having a high grinding force. Accordingly, the polishing film can be suitably used in the finishing process of the connection end face of the optical fiber connector, for example.
- a polishing film 1 shown in FIG. 1 has a sheet-like substrate 10 and a polishing layer 20 laminated on the surface thereof.
- the material of the substrate 10 is not particularly limited, but a material that has appropriate rigidity and ensures good adhesion and adhesion with the polishing layer 20 is preferable.
- a known thermoplastic resin can be used, and examples thereof include acrylic resin, polycarbonate, polyethylene terephthalate (PET), polypropylene (PP), and polyethylene (PE).
- PET polyethylene terephthalate
- PP polypropylene
- PE polyethylene
- a biaxially stretched film such as PET, PP, or PE may be used.
- the process which improves adhesiveness such as a chemical process, a corona process, and a primer process, may be performed on the surface of the base material 10.
- the planar shape and size of the substrate 10 are not particularly limited, but may be, for example, a 127 mm ⁇ 127 mm square shape or a 127 mm diameter circular shape. Moreover, the structure by which the several base material 10 juxtaposed on the plane is supported by a single support body may be sufficient.
- the average thickness of the substrate 10 is not particularly limited, but can be, for example, 30 ⁇ m or more and 150 ⁇ m or less.
- the average thickness of the base material 10 is less than the lower limit, the strength and flatness of the polishing film may be insufficient.
- the average thickness of the base material 10 exceeds the upper limit, the polishing film is unnecessarily thick and may be difficult to handle.
- the polishing layer 20 is laminated on the surface of the substrate 10 and has a resin binder 21 and abrasive particles 22 dispersed in the resin binder 21.
- the lower limit of the average thickness of the polishing layer 20 is preferably 4 ⁇ m and more preferably 5 ⁇ m. Further, the upper limit of the average thickness of the polishing layer 20 is preferably 15 ⁇ m, and more preferably 12 ⁇ m. When the average thickness of the polishing layer 20 is less than the lower limit, the abrasion resistance of the polishing film may be insufficient. On the other hand, when the average thickness of the polishing layer 20 exceeds the upper limit, it may be difficult to control the amount of optical fiber drawn during polishing.
- the indentation hardness of the polishing layer 20 exceeds the upper limit, the optical fiber is selectively polished at the time of polishing, and the optical fiber may be drawn into the ferrule.
- the indentation hardness of the polishing layer 20 is less than the lower limit, the grinding force of the polishing film may be insufficient.
- polishing of the connection end face of the optical fiber connector is performed by pressing the connection end face of the optical fiber connector with a load against a polishing film attached to the surface of the elastic pad.
- the polishing pressure near the apex of the optical fiber connector formed on the spherical surface increases, so that the optical fiber near the apex of the optical fiber connector is selectively polished, and the optical fiber with respect to the ferrule It is thought that pulling in will occur. Therefore, by reducing the indentation hardness of the polishing layer 20, it is considered that the followability of the polishing layer 20 to the elastic pad becomes high, and the optical fiber can be controlled stably and accurately.
- the present inventors conducted the following tests to confirm the optimum range of the indentation hardness of the polishing layer 20 that has a high grinding force and can control the drawing of the optical fiber stably and accurately. .
- the content of abrasive particles 22 having a primary particle diameter of 70 nm or more with respect to the entire abrasive particles 22 is 10% by mass or more and 50% by mass or less, and the content of abrasive particles 22 in the polishing layer 20
- Five types of polishing films having a mass of 84% by mass or more were prepared, and the indentation hardness of these abrasive films was measured using a microindentation hardness tester (“ENT-1100a” manufactured by Elionix Co., Ltd.).
- this polishing film is punched into a 127 mm diameter circular shape and fixed by attaching to an elastic pad (hardness 70 °) of a polishing machine (“SFP-550S” by Seiko Giken Co., Ltd.) to polish ion exchange water.
- the final finish polishing was performed for 60 seconds at a rotation speed of 1 rpm for rotation and 70 rpm for rotation on the connection end face of the optical fiber connector after intermediate finish polishing.
- the amount of the optical fiber connector pulled in after polishing was measured using an optical connector end face three-dimensional shape measuring machine (“ACCIS NC / AC-3000” manufactured by Norland). When the optical fiber protrudes from the ferrule, the pull-in amount is expressed as a negative value.
- the pull-in amount of the optical connector has a correlation with the indentation hardness of the polishing film.
- the amount of the optical fiber drawn can be ⁇ 10 nm or less.
- the pull-in amount is preferably ⁇ 30 nm to ⁇ 10 nm from the viewpoint of light loss. Therefore, by setting the indentation hardness of the polishing film to 370 N / mm 2 or less, it has a high grinding force and is stable and accurate. It is considered that the pull-in of the optical fiber can be controlled.
- a resin or an elastomer can be used as the main component of the resin binder 21, a resin or an elastomer can be used.
- the resin include acrylic resin, epoxy resin, cellulose resin, polyvinyl, phenoxy resin, phenol resin, and polyester.
- the elastomer include styrene, olefin, ester, urethane, amide, polyvinyl chloride (PVC), fluorine thermoplastic elastomer, natural rubber, styrene-butadiene rubber, isoprene rubber, butadiene.
- the resin examples thereof include rubber, chloroprene rubber, acrylonitrile-butadiene rubber, butyl rubber, ethylene-propylene rubber, ethylene-propylene-diene rubber, acrylic rubber, and silicone rubber.
- the resin is the main component, an acrylic resin, an epoxy resin, and a polyester that can easily ensure good dispersibility of the abrasive particles 22 and good adhesion to the substrate 10 are preferable.
- urethane-based thermoplastic elastomers, amide-based thermoplastic elastomers, acrylonitrile-butadiene rubber, urethane rubber and acrylic rubber are preferred.
- the resin may be at least partially crosslinked and may contain a curing agent such as polyisocyanate or acrylate.
- the “main component” means a component having the highest content, for example, a component having a content of 50% by mass or more.
- auxiliary agents such as resins other than the main components, crosslinking agents, dispersing agents, coupling agents, surfactants, lubricants, antifoaming agents, and coloring agents, additives, and the like are used depending on the purpose. You may make it contain suitably.
- the resin binder 21 may further contain an elastomer.
- polishing layer 20 can be made low because the resin binder 21 contains an elastomer.
- the upper limit of the glass transition temperature of the elastomer is preferably 20 ° C, more preferably 15 ° C.
- the elastomer may be in a glass state when the optical fiber connector is polished, and the polishing layer 20 may be cured.
- the same elastomer as the main component can be used.
- the content of the above-mentioned elastomer to resin binder 21 20 mass% is preferred and 30 mass% is more preferred.
- an upper limit of content of the said elastomer with respect to the resin binder 21 75 mass% is preferable and 50 mass% is more preferable.
- the content of the elastomer relative to the resin binder 21 is less than the lower limit, it may be difficult to control the indentation hardness of the polishing layer 20.
- the content of the elastomer with respect to the resin binder 21 exceeds the upper limit, the dispersibility of the abrasive particles 22 in the resin binder 21 may be insufficient.
- abrasive particles 22 examples include particles of diamond, alumina, silica, and the like. Among these, silica particles that can provide a high grinding force are preferable. Examples of the silica particles include known silica particles such as colloidal silica, dry silica, wet silica, and fused silica.
- colloidal silica includes an organosilica sol in which colloidal silica is dispersed in an organic solvent.
- the abrasive particles 22 include abrasive particles having a primary particle diameter of 70 nm or more (large-diameter abrasive particles 22a) and abrasive particles having a primary particle diameter of less than 70 nm (small-diameter abrasive particles 22b). Since the abrasive particles 22 include large-diameter abrasive particles 22a, the abrasive film has a high grinding force. Further, since the abrasive particles 22 include small-diameter abrasive particles 22b, the abrasive film has high polishing accuracy.
- the primary particle size distribution of the abrasive particles 22 it is preferable to have one maximum value (peak) in the range of less than 70 nm and in the range of 70 nm or more.
- peak the polishing film can easily and reliably have high polishing accuracy obtained by the small-diameter abrasive particles 22b and high grinding force obtained by the large-diameter abrasive particles 22a. it can.
- the lower limit of the minimum primary particle diameter of the abrasive particles 22 is preferably 1 nm, and more preferably 10 nm.
- the upper limit of the maximum primary particle size of the abrasive particles 22 is preferably 400 nm, and more preferably 300 nm.
- the polishing time of the connection end face of the optical fiber connector may increase.
- the maximum value of the particle diameter of the abrasive particles 22 exceeds the upper limit, it may be difficult to control the drawing of the optical fiber during polishing.
- the lower limit of the content of the large-diameter abrasive particles 22a with respect to the entire abrasive particles 22 is 10% by mass, and more preferably 25% by mass.
- an upper limit of content of the large diameter abrasive particle 22a with respect to the whole said abrasive particle 22 it is 50 mass%, and 35 mass% is more preferable.
- the content of the large-diameter abrasive particles 22a with respect to the entire abrasive particles 22 is less than the lower limit, the grinding force of the abrasive film may be insufficient.
- the content of the large-diameter abrasive particles 22a with respect to the entire abrasive particles 22 exceeds the above upper limit, it may be difficult to control the pull-in amount of the optical fiber during polishing.
- the lower limit of the content of the abrasive particles 22 with respect to the polishing layer 20 is 84% by mass, and more preferably 87% by mass. Moreover, as an upper limit of content of the abrasive particle 22 with respect to the said grinding
- the manufacturing method of the said polishing film can employ
- a solution in which the resin binder 21 and the abrasive particles 22 are dispersed in a solvent is prepared as a coating liquid.
- the solvent is not particularly limited as long as the resin binder 21 is soluble. Specifically, methyl ethyl ketone (MEK), isophorone, terpineol, N methylpyrrolidone, cyclohexanone, propylene carbonate, or the like can be used.
- MEK methyl ethyl ketone
- isophorone isophorone
- terpineol N methylpyrrolidone
- cyclohexanone propylene carbonate
- a diluent such as water, alcohol, ketone, acetate ester and aromatic compound may be added.
- auxiliaries and additives may be mixed.
- the coating liquid prepared in the coating liquid preparation process is applied to the surface of the substrate 10.
- the coating method is not particularly limited, and for example, known coating methods such as bar coating, comma coating, spray coating, reverse roll coating, knife coating, screen printing, gravure coating, and die coating can be used.
- the applied coating liquid is dried and reaction-cured to form the polishing layer 20.
- the solvent of the coating liquid is evaporated and the solute is cured, thereby forming the polishing layer 20.
- the abrasive film has an indentation hardness of the abrasive layer 20 of 370 N / mm 2 or less, and the content of the large abrasive particles 22 a having a primary particle diameter of 70 nm or more with respect to the entire abrasive particles 22 is 50 mass% or less. Later pulling of the optical fiber can be prevented. Moreover, since the content of the large-diameter abrasive particles 22a with respect to the entire abrasive particles is 10% by mass or more and the content of the abrasive particles 22 in the abrasive layer 20 is 84% by mass or more, the abrasive film has high grinding. Have power.
- the present invention is not limited to the above-described embodiment, and can be implemented in a mode in which various changes and improvements are made in addition to the above-described mode.
- the polishing film in which the polishing layer is directly formed on the surface of the substrate has been described.
- the primer treatment layer for ensuring the adhesion between the substrate and the polishing layer between the substrate and the polishing layer. May be provided.
- the main component of the primer-treated layer is not particularly limited as long as the adhesion between the substrate and the polishing layer can be secured.
- water-soluble or water-dispersible polyester or acrylic resin, water-soluble or water-soluble A resin obtained by grafting an unsaturated bond-containing compound to a dispersible hydrophilic group-containing polyester can be used.
- the primer-treated layer can be formed, for example, by spray-coating a primer agent containing the main component on the surface of the substrate and then drying. Moreover, you may use the base material by which the primer process layer was previously provided on the surface of the base material.
- the polishing layer may have a groove.
- a lattice shape at equal intervals or a stripe shape in which a plurality of linear grooves are arranged substantially in parallel can be used. Since the polishing layer has a groove, polishing debris and the like generated during polishing can be efficiently removed.
- Example 1 250 parts by mass of organosilica sol (“MEK-ST”, Nissan Chemical Industries, Ltd., primary particle size 10-20 nm, solid content 30% by mass) as small abrasive particles, fused silica (electrochemical industry) as large abrasive particles Tetrahiro which contains 10 parts by mass of “UFP-30”, an average primary particle size of 99 nm), and 5% by mass of a crosslinked urethane-based thermoplastic elastomer as a resin binder (“Kuramylon U9180” of Kuraray Co., Ltd.) 220 parts by mass of a solution of Drofuran, 5 parts by mass of polyisocyanate (“Desmodur L75C” from Sumika Bayer Urethane Co., Ltd., solid content: 75% by mass) as a resin binder, and 33 parts by mass of methyl ethyl ketone as a solvent are mixed. A coating solution was obtained.
- organosilica sol (“MEK-ST”, Nissan Chemical Industries
- Example 2 207 parts by mass of organosilica sol (Nissan Chemical Co., Ltd. “MEK-ST”, primary particle size 10-20 nm, solid content 30% by mass) as small abrasive particles, and organosilica sol (Nissan Chemical Industries as large abrasive particles) 87 parts by mass of “IPA-ST-ZL”, primary particle size 70-100 nm, solid content 30% by mass, vulcanized acrylonitrile-butadiene rubber as resin binder (“N230S” by JSR Corporation) 60 parts by mass of N, N-dimethylformamide solution containing 5% by mass of cellulose, 60 parts by mass of methyl ethyl ketone containing 5% by mass of cellulose resin (Nisshinsei Co., Ltd.
- Etocel 100 as a resin binder and resin Polyisocyanate as binder ("Death Module L” from Sumika Bayer Urethane Co., Ltd. 5C ", the solid content 75 mass%) 7 parts by weight were mixed to obtain a coating solution.
- the above coating solution is applied to one surface of a polyester film (“HLE-75” manufactured by Teijin DuPont Films Ltd., average thickness: 75 ⁇ m) as a base material using a bar coating method and dried at 100 ° C. in an oven.
- a polishing film having a polishing layer having an average thickness of 6 ⁇ m was obtained.
- the content of abrasive particles in this polishing layer is 88% by mass.
- Organosilica sol as a small abrasive particle (“MEK-ST” from Nissan Chemical Industries, Ltd., primary particle diameter 10-20 nm, solid content 30% by mass) 210 parts by mass
- Organosilica sol as a large abrasive particle (Nissan Chemical Industry) 87 parts by mass of “IPA-ST-ZL”, primary particle size 70-100 nm, solid content 30% by mass
- vulcanized acrylonitrile-butadiene rubber as resin binder (“N230S” by JSR Corporation) 100 parts by mass of N, N-dimethylformamide solution containing 5% by mass of polyisocyanate and 7 parts by mass of polyisocyanate as a resin binder (“Desmodur L75C” from Sumika Bayer Urethane Co., Ltd., solid content: 75% by mass)
- a coating solution was obtained.
- the above coating solution is applied to one surface of a polyester film (“HLE-75” manufactured by Teijin DuPont Films Ltd., average thickness: 75 ⁇ m) as a base material using a bar coating method and dried at 100 ° C. in an oven.
- a polishing film having a polishing layer having an average thickness of 11 ⁇ m was obtained.
- the content of abrasive particles in this polishing layer is 90% by mass.
- Organosilica sol (“IPA-ST”, Nissan Chemical Industries, Ltd., primary particle size 10-20 nm, solid content 30% by mass) as small-diameter abrasive particles 240 parts by mass, wet silica as large-diameter abrasive particles (Fuso Chemical Industries) 140 parts of 2-propanol solution containing 18 parts by mass of “SP03F”, an average primary particle size of 300 nm, and 5% by mass of a crosslinked acrylic elastomer (“BR102” of Mitsubishi Rayon Co., Ltd.) as a resin binder.
- IPA-ST Nissan Chemical Industries, Ltd., primary particle size 10-20 nm, solid content 30% by mass
- wet silica as large-diameter abrasive particles (Fuso Chemical Industries) 140 parts of 2-propanol solution containing 18 parts by mass of “SP03F”, an average primary particle size of 300 nm, and 5% by mass of a crosslinked acrylic elastomer (“BR102” of Mitsubishi Ray
- the above coating solution is applied to one surface of a polyester film (“HLE-75” manufactured by Teijin DuPont Films Ltd., average thickness: 75 ⁇ m) as a base material using a bar coating method and dried at 100 ° C. in an oven.
- a polishing film having a polishing layer having an average thickness of 5 ⁇ m was obtained.
- the content of abrasive particles in this polishing layer is 90% by mass.
- the company “UFP-30”, average primary particle size 99 nm) was 7.5 parts by mass, and the resin binder and solvent were the same as in Example 1 except that the same coating solution as in Example 1 was used.
- a polishing film having a polishing layer having a thickness of 5 ⁇ m was obtained. The content of abrasive particles in this polishing layer is 80% by mass.
- the above coating solution is applied to one surface of a polyester film (“HLE-75” manufactured by Teijin DuPont Films Ltd., average thickness: 75 ⁇ m) as a base material using a bar coating method and dried at 100 ° C. in an oven.
- a polishing film having a polishing layer having an average thickness of 5 ⁇ m was obtained.
- the content of abrasive particles in this polishing layer is 85% by mass.
- Example 3 147 parts by mass of organosilica sol (Nissan Chemical Industry Co., Ltd. “MEK-ST”, primary particle size 10-20 nm, solid content 30 mass%) as small-diameter abrasive particles and large-diameter abrasive particles (Nissan Chemical Industries) Example except that “IPA-ST-ZL”, a primary particle size of 70 to 100 nm, solid content of 30% by mass) was 153 parts by mass, and the resin binder was the same coating solution as in Example 3. In the same manner as in Example 3, an abrasive film having an abrasive layer having an average thickness of 5 ⁇ m was obtained. The content of abrasive particles in this polishing layer is 90% by mass.
- polishing conditions Using the polishing films obtained in Examples 1 to 4 and Comparative Examples 1 to 4, an optical fiber connector in which an optical fiber was bonded to a ferrule (“SC Ferrule” of Seiko Giken Co., Ltd.) was polished. First, the polishing film is punched into a 127 mm diameter circular shape and fixed by attaching to an elastic pad (hardness 70 °) of a polishing machine (“SFP-550S” by Seiko Giken Co., Ltd.), and ion-exchanged water is used as a polishing liquid. The final finish polishing was performed on the connection end face of the optical fiber connector after the intermediate finish polishing for 60 seconds at a rotation speed of 1 rpm for rotation and 70 rpm for rotation.
- the intermediate finish polishing is performed by using a polishing film (“TOPXD105” manufactured by Bando Chemical Co., Ltd.) having diamond abrasive grains having an average primary particle size of 1 ⁇ m, and an elasticity of a polishing machine (“SFP-550S” manufactured by Seiko Giken Co., Ltd.). Affixed to a body pad (hardness 80 °), ion-exchanged water is used as the polishing liquid, and final finish polishing is performed on the connection end face of the optical fiber connector after rough spherical polishing at a rotation speed of 1 rpm and revolution 70 rpm. For a second.
- ⁇ Retraction amount> The pull-in amount of the optical fiber connector after polishing was measured using an optical connector end face three-dimensional shape measuring instrument (“ACCIS NC / AC-3000” manufactured by Norland). When the optical fiber protrudes from the ferrule, the pull-in amount is expressed as a negative value. Further, since the amount of entrainment is preferably from ⁇ 30 nm to ⁇ 10 nm from the viewpoint of light loss, the measured value was determined according to the following criteria. A: The pull-in amount is in the range of ⁇ 30 nm to ⁇ 10 nm. B: The amount of drawing is outside the range of ⁇ 30 nm to ⁇ 10 nm.
- End face condition The state of the end face was observed using “Video Fiber Microscope” manufactured by Westover Corporation, and judged according to the following criteria. A: Deposits and scratches are not found, and a good end surface is obtained. B: Deposits or scratches are observed, and a good end face cannot be obtained.
- the content of the large-diameter abrasive particles exceeds 50% by mass, so that the pull-in amount of the optical fiber cannot be controlled.
- Comparative Example 4 since the indentation hardness of the polishing layer exceeds 370 N / mm 2 , the optical fiber is selectively polished at the time of polishing, and the pulling amount of the optical fiber is larger than ⁇ 10 nm. That is, in the abrasive films of Examples 1 to 4, the content of abrasive particles having a primary particle diameter of 70 nm or more with respect to the entire abrasive particles is 10% by mass or more and 50% by mass or less, and the content of the abrasive particles in the polishing layer is 84. Since the indentation hardness of the polishing layer is 370 N / mm 2 or less, it is possible to prevent the optical fiber from being pulled after polishing.
- the polishing film of the present invention can prevent pulling of the optical fiber after polishing while having a high grinding force. Accordingly, the polishing film can be suitably used in the finishing process of the connection end face of the optical fiber connector, for example.
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Abstract
Description
図1に示す研磨フィルム1は、シート状の基材10と、その表面に積層される研磨層20とを有する。
上記基材10の材質としては、特に限定されないが、適度な剛性を有し、研磨層20との良好な接着性や密着性が確保される材質が好ましい。このような材質としては、公知の熱可塑性樹脂を用いることができ、例えばアクリル樹脂、ポリカーボネート、ポリエチレンテレフタレート(PET)、ポリプロピレン(PP)、ポリエチレン(PE)等が挙げられる。基材10として、PET、PP、PE等の二軸延伸フィルムを用いてもよい。また、基材10の表面に化学処理、コロナ処理、プライマー処理等の接着性を高める処理が行われてもよい。
上記研磨層20は、基材10の表面に積層され、樹脂バインダー21及びこの樹脂バインダー21中に分散される研磨粒子22を有する。
上記樹脂バインダー21の主成分としては、樹脂又はエラストマーを用いることができる。上記樹脂としては、例えばアクリル樹脂、エポキシ樹脂、セルロース樹脂、ポリビニル、フェノキシ樹脂、フェノール樹脂、ポリエステル等を挙げることができる。また、上記エラストマーとしては、例えばスチレン系、オレフィン系、エステル系、ウレタン系、アミド系、ポリ塩化ビニル(PVC)系、フッ素系の熱可塑性エラストマー、天然ゴム、スチレン-ブタジエンゴム、イソプレンゴム、ブタジエンゴム、クロロプレンゴム、アクリロニトリル-ブタジエンゴム、ブチルゴム、エチレン-プロピレンゴム、エチレン-プロピレン-ジエンゴム、アクリルゴム、シリコーンゴム等を挙げることができる。樹脂を主成分とする場合、研磨粒子22の良好な分散性と基材10への良好な密着性とが確保しやすいアクリル樹脂、エポキシ樹脂及びポリエステルが好ましく、エラストマーを主成分とする場合、基材10への密着性と取扱い性の観点からウレタン系熱可塑性エラストマー、アミド系熱可塑性エラストマー、アクリロニトリル-ブタジエンゴム、ウレタンゴム及びアクリルゴムが好ましい。また、上記樹脂は、少なくとも一部が架橋していてもよく、ポリイソシアネート、アクリレート等の硬化剤を含有してもよい。ここで「主成分」とは、最も含有量の多い成分を意味し、例えば含有量が50質量%以上の成分をいう。
上記研磨粒子22としては、ダイヤモンド、アルミナ、シリカ等の粒子が挙げられる。中でも高い研削力が得られるシリカ粒子が好ましい。このシリカ粒子としては、例えばコロイダルシリカ、乾式シリカ、湿式シリカ、溶融シリカ等の公知のシリカ粒子を用いることができる。ここで、「コロイダルシリカ」は、コロイダルシリカを有機溶媒に分散させたオルガノシリカゾルを含むものとする。
当該研磨フィルムの製造方法は、基材10と研磨層20との接着性及び密着性を十分に確保できる公知の薄膜製造技術を採用することができ、例えば塗工液を準備する工程、上記塗工液を基材10表面に塗布する工程及び塗布した塗工液を乾燥する工程を備える。
当該研磨フィルムは、研磨層20の押し込み硬さが370N/mm2以下であり、研磨粒子22全体に対する一次粒子径70nm以上の大径研磨粒子22aの含有量が50質量%以下であるので、研磨後の光ファイバの引き込みを防止できる。また、当該研磨フィルムは、研磨粒子全体に対する大径研磨粒子22aの含有量が10質量%以上であり、上記研磨層20における上記研磨粒子22の含有量が84質量%以上であるので、高い研削力を有する。
本発明は上記実施形態に限定されるものではなく、上記態様の他、種々の変更、改良を施した態様で実施することができる。
小径研磨粒子としてのオルガノシリカゾル(日産化学工業株式会社の「MEK-ST」、一次粒子径10~20nm、固形分30質量%)を250質量部、大径研磨粒子としての溶融シリカ(電気化学工業株式会社の「UFP-30」、平均一次粒子径99nm)を10質量部、樹脂バインダーとしての架橋済のウレタン系熱可塑性エラストマー(株式会社クラレの「クラミロンU9180」)を5質量%含有するテトラヒロドロフラン溶解液を220質量部、樹脂バインダーとしてのポリイソシアネート(住化バイエルウレタン株式会社の「デスモジュールL75C」、固形分75質量%)を5質量部及び溶剤としてのメチルエチルケトンを33質量部混合し、塗布液を得た。
小径研磨粒子としてのオルガノシリカゾル(日産化学工業株式会社の「MEK-ST」、一次粒子径10~20nm、固形分30質量%)を207質量部、大径研磨粒子としてのオルガノシリカゾル(日産化学工業株式会社の「IPA-ST-ZL」、一次粒子径70~100nm、固形分30質量%)を87質量部、樹脂バインダーとしての加硫済のアクリロニトリル-ブタジエンゴム(JSR株式会社の「N230S」)を5質量%含有するN,N-ジメチルホルムアミド溶解液を60質量部、樹脂バインダーとしてのセルロース樹脂(日進化成株式会社の「エトセル100」)を5質量%含有するメチルエチルケトンを60質量部及び樹脂バインダーとしてのポリイソシアネート(住化バイエルウレタン株式会社の「デスモジュールL75C」、固形分75質量%)を7質量部混合し、塗布液を得た。
小径研磨粒子としてのオルガノシリカゾル(日産化学工業株式会社の「MEK-ST」、一次粒子径10~20nm、固形分30質量%)を210質量部、大径研磨粒子としてのオルガノシリカゾル(日産化学工業株式会社の「IPA-ST-ZL」、一次粒子径70~100nm、固形分30質量%)を87質量部、樹脂バインダーとしての加硫済のアクリロニトリル-ブタジエンゴム(JSR株式会社の「N230S」)を5質量%含有するN,N-ジメチルホルムアミド溶解液を100質量部及び樹脂バインダーとしてのポリイソシアネート(住化バイエルウレタン株式会社の「デスモジュールL75C」、固形分75質量%)を7質量部混合し、塗布液を得た。
小径研磨粒子としてのオルガノシリカゾル(日産化学工業株式会社の「IPA-ST」、一次粒子径10~20nm、固形分30質量%)を240質量部、大径研磨粒子としての湿式シリカ(扶桑化学工業株式会社の「SP03F」、平均一次粒子径300nm)を18質量部、樹脂バインダーとしての架橋済のアクリルエラストマー(三菱レイヨン株式会社の「BR102」)を5質量%含有する2-プロパノール溶解液を140質量部、樹脂バインダーとしてのポリイソシアネート(住化バイエルウレタン株式会社の「デスモジュールL75C」、固形分75質量%)を4質量部及び溶剤としてのメチルエチルケトンを50質量部混合し、塗布液を得た。
小径研磨粒子としてのオルガノシリカゾル(日産化学工業株式会社の「MEK-ST」、一次粒子径10~20nm、固形分30質量%)を175質量部及び大径研磨粒子として溶融シリカ(電気化学工業株式会社の「UFP-30」、平均一次粒子径99nm)を7.5質量部とし、樹脂バインダー及び溶剤は実施例1と同様とした塗布液を用いた以外は、実施例1と同様にして平均厚さ5μmの研磨層を有する研磨フィルムを得た。この研磨層の研磨粒子の含有量は80質量%である。
小径研磨粒子としてのオルガノシリカゾル(日産化学工業株式会社の「MEK-ST」、一次粒子径10~20nm、固形分30質量%)を267質量部、大径研磨粒子としてのオルガノシリカゾル(日産化学工業株式会社の「IPA-ST-ZL」、一次粒子径70~100nm、固形分30質量%)を17質量部、樹脂バインダーとしてのアクリロニトリル-ブタジエンゴム(JSR株式会社の「N230S」)を5質量%含有するN,N-ジメチルホルムアミド溶解液を60質量部、樹脂バインダーとしてのセルロース樹脂(日進化成株式会社の「エトセル100」)を120質量部及び樹脂バインダーとしてのポリイソシアネート(住化バイエルウレタン株式会社の「デスモジュールL75C」、固形分75質量%)を8質量部混合し、塗布液を得た。
小径研磨粒子としてのオルガノシリカゾル(日産化学工業株式会社の「MEK-ST」、一次粒子径10~20nm、固形分30質量%)を147質量部及び大径研磨粒子としてのオルガノシリカゾル(日産化学工業株式会社の「IPA-ST-ZL」、一次粒子径70~100nm、固形分30質量%)を153質量部とし、樹脂バインダーは実施例3と同様とした塗布液を用いた以外は、実施例3と同様にして平均厚さ5μmの研磨層を有する研磨フィルムを得た。この研磨層の研磨粒子の含有量は90質量%である。
樹脂バインダーとしてセルロース樹脂(日進化成株式会社の「エトセル100」)を5質量%含有するメチルエチルケトンを120質量部及びポリイソシアネート(住化バイエルウレタン株式会社の「デスモジュールL75C」、固形分75質量%)を8質量部とし、研磨粒子は実施例2と同様とした塗布液を用いた以外は、実施例2と同様にして平均厚さ6μmの研磨層を有する研磨フィルムを得た。この研磨層の研磨粒子の含有量は88質量%である。
上記実施例1~4及び比較例1~4で得られた研磨フィルムを用いて、フェルール(株式会社精工技研の「SCフェルール」)に光ファイバが接着された光ファイバコネクタの研磨を行った。まず、研磨フィルムを直径127mmの円型に打ち抜き、研磨機(株式会社精工技研の「SFP-550S」)の弾性体パッド(硬度70°)に貼り付けて固定し、イオン交換水を研磨液として用い、中間仕上げ研磨後の光ファイバコネクタの接続端面に対し最終仕上げ研磨を自転1rpm、公転70rpmの回転数で60秒間行った。
研磨した光ファイバコネクタについて、以下の評価を行った。結果を表1に示す。
研磨後の光ファイバコネクタの引き込み量は、光コネクタ端面三次元形状測定機(Norland社の「ACCIS NC/AC-3000」)を用いて計測した。なお、フェルールに対し光ファイバが突き出した状態となる場合は、引き込み量を負値として表す。また、引き込み量として光損失の観点より-30nm以上-10nm以下が好ましいことから、計測値については以下の判断基準で判定した。
A:引き込み量が-30nm以上-10nm以下の範囲内である。
B:引き込み量が-30nm以上-10nm以下の範囲外である。
端面の状態は、WESTOVER社の「Video Fiber Microscope」を用いて観察し、以下の判断基準で判定した。
A:付着物及びスクラッチが見受けられず、良好な端面が得られる。
B:付着物又はスクラッチが見受けられ、良好な端面が得られない。
20 研磨層
21 樹脂バインダー
22 研磨粒子
22a 大径研磨粒子
22b 小径研磨粒子
Claims (4)
- 基材と、その表面側に積層される研磨層とを有する研磨フィルムであって、
上記研磨層が、樹脂バインダー及びこの樹脂バインダー中に分散される研磨粒子を有し、
上記研磨粒子全体に対する一次粒子径70nm以上の研磨粒子の含有量が10質量%以上50質量%以下であり、
上記研磨層における上記研磨粒子の含有量が84質量%以上であり、
上記研磨層の押し込み硬さが370N/mm2以下であることを特徴とする研磨フィルム。 - 上記研磨粒子が、シリカ粒子である請求項1に記載の研磨フィルム。
- 上記研磨層の平均厚さが4μm以上15μm以下である請求項1に記載の研磨フィルム。
- 上記樹脂バインダーが、ガラス転移温度20℃以下のエラストマーを含有し、
上記樹脂バインダーに対する上記エラストマーの含有量が20質量%以上である請求項1に記載の研磨フィルム。
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EP3168002B1 (en) | 2022-03-23 |
KR101904732B1 (ko) | 2018-10-05 |
CN106470800B (zh) | 2019-06-18 |
JP5921790B1 (ja) | 2016-05-24 |
CN106470800A (zh) | 2017-03-01 |
US10543582B2 (en) | 2020-01-28 |
EP3168002A1 (en) | 2017-05-17 |
KR20170016443A (ko) | 2017-02-13 |
JPWO2016006476A1 (ja) | 2017-04-27 |
EP3168002A4 (en) | 2018-08-22 |
US20170157745A1 (en) | 2017-06-08 |
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