Classifications

• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09G—POLISHING COMPOSITIONS; SKI WAXES
  • C09G1/00—Polishing compositions
  • C09G1/02—Polishing compositions containing abrasives or grinding agents
• • 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
• • 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
• • 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
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
  • C09K3/00—Materials not provided for elsewhere
  • C09K3/14—Anti-slip materials; Abrasives

Definitions

• the present invention relates to an abrasive for ferrules used for polishing the end faces of ferrules.
• optical fiber used as a means of transmission for optical communications is required to have as little optical loss as possible in line with the recent demand for higher capacity and higher efficiency.
• Optical connectors are used to connect optical fibers to each other.
• the optical connector has a ferrule.
• the ferrule has an insertion hole through which an optical fiber is inserted.
• the optical fiber is fixed to the ferrule with an adhesive or the like.
• connection end face of the optical connector is extremely important as it affects the optical characteristics of the optical fiber. Therefore, the end face of the optical connector is mirror-finished by a plurality of stages of polishing. As the final finishing of polishing, precise mirror polishing is performed using abrasive materials such as polishing sheets, polishing tapes, polishing whetstones, and polishing cloths each having a polishing layer containing fine abrasive grains (Patent Document 1).
• abrasive materials such as polishing sheets, polishing tapes, polishing whetstones, and polishing cloths each having a polishing layer containing fine abrasive grains
• a multicore optical fiber has been developed in which a plurality of optical fibers are bundled together.
• a multi-core ferrule is used for connecting multi-core optical fibers, and its end faces are required to be more precisely mirror-finished.
• a plurality of ferrules may be polished at the same time in order to improve workability, and precision mirror finishing is required as with multi-core ferrules.
• the abrasive has high durability and less deterioration due to use. Furthermore, when the deterioration of the abrasive is small, the abrasive can be used continuously, and the workability is improved.
• the present invention has been completed in view of the above circumstances, and an object to be solved is to provide a high-performance polishing material for ferrules suitable for polishing ferrules.
• the height of the plurality of optical fibers is higher than a predetermined value and uniform after polishing, and a uniform polishing state is achieved with a little polishing. is required. It is also required that the polished surface should not be scratched and that the generation of core dips in the core constituting the optical fiber should be suppressed.
• the height of the optical fiber was solved by containing abrasive grains with a small particle size, and suppression of core dip was achieved by using silica as abrasive grains. This was resolved by adopting the Further, the inventors have found that the surface can be polished without damage by increasing the amount of abrasive grains and containing abrasive grains of a certain size. Furthermore, the inventors have found that the durability can be improved by adopting an epoxy resin as a binder for holding the abrasive.
• the abrasive material for ferrules of the present invention which solves the above problems, has a binder made of a resin material and abrasive grains dispersed in the binder. All of the resin materials are crosslinked.
• the abrasive grains are contained in an amount of 80% or more and 91% or less based on the sum of the mass of the abrasive grains and the binder, and 62 small-diameter particles that are particles with a particle size of 100 nm or less based on the mass of the abrasive grains. 0.5% or more and 80% or less, and composed of silica.
• the epoxy resin is preferably of biphenyl type.
• the binder preferably has a pencil hardness of 3H or higher.
• the small-diameter particles are preferably particles having a peak top particle size of 50 nm or less. By controlling the height within this range, it becomes easier to achieve a uniform height of the optical fiber.
• the abrasive grains contain particles having a peak top particle diameter of 150 nm or more, because it becomes easy to keep the surface condition free from scratches after polishing.
• the polishing material for ferrules of the present invention has the above-described structure, so that the polishing performance of ferrules is high and durability can also be improved.
• the ferrule polishing material of this embodiment is a member for polishing the end face of a ferrule.
• a ferrule is a member for terminating optical fibers, and is a member that constitutes an optical connector that connects optical fibers.
• the abrasive material for ferrules of this embodiment consists of abrasive grains, a binder for dispersing the abrasive grains, and other necessary members. It is preferable to use a polishing layer in which abrasive grains and a binder for dispersing the abrasive grains are formed in layers.
• the thickness is preferably 5 ⁇ m or less, more preferably 3 ⁇ m or less. Reducing the thickness improves the durability of the polishing layer.
• the abrasive grains are contained in an amount of 80% or more and 91% or less based on the sum of the mass of the abrasive grains and the binder.
• lower limits of 85%, 86%, 87% and 87.5% can be used, and upper limits of 90%, 89%, 88% and 87.5% can be used. These upper and lower limits can be combined arbitrarily.
• Abrasive grains are composed of silica. Although materials other than silica can be mixed, the amount of silica is preferably 95% or more, more preferably 97.5% or more, and further 99% or more based on the mass of the entire abrasive grain. is more preferable.
• the material other than silica can be contained as particles separate from particles made of silica, or can be contained in the same particles as silica.
• the particle size distribution of abrasive grains is specified. Specifically, 62.5% or more and 80% or less of small-diameter particles are present based on the mass of the entire abrasive grains. 65%, 70%, 72.5%, and 75% can be adopted as the lower limit of the abundance of small-diameter particles. As the upper limit, 79%, 78%, 77%, 76% and 75% can be adopted. These upper and lower limits can be combined arbitrarily. Small-diameter particles are particles having a particle size below a certain particle size. Particles having a particle size of 0.1 ⁇ m or less, preferably 30 nm or less, and more preferably 20 nm or less are used as a certain particle size.
• the small-diameter particles have a peak top at a particle size below the above-described certain particle size.
• the peak top means having a peak when the particle size distribution is expressed on a volume basis, and the particle size at the peak top indicates the particle size at the peak.
• the particle diameter at the peak top is preferably a mode diameter within the range of particle diameters below a certain particle diameter.
• the peak top particle size of the small-diameter particles is preferably 50 nm or less, more preferably 30 nm or less, and more preferably 20 nm or less.
• abrasive grains is not particularly limited, but spherical spherical silica, crushed crushed silica, etc. can be used. Moreover, it is preferable to contain particles having a particle size of 100 nm or more. In particular, it has a peak top, and the particle size at the peak top is preferably 150 nm or more, more preferably 200 nm or more. Furthermore, it is desirable not to contain particles with a particle size of 5 ⁇ m or more in order to suppress scratches on the polished surface. It preferably contains crushed silica.
• particle size means a laser diffraction/scattering particle size distribution analyzer (LA-750: manufactured by HORIBA, Ltd.) and a dynamic light scattering Nanotrack particle size distribution analyzer (UPA-EX150: manufactured by Nikkiso Co., Ltd.). is a value measured by combining
• a large particle size range can be measured.
• the particle size of particles having a particle size of 100 nm or less is confirmed by batch measurement using a particle size distribution meter in a state of being dispersed in methyl ethyl ketone. Particle size distribution is measured by combining the measurement results of both.
• Spherical silica can be produced by reacting metal silicon with oxygen.
• Spherical silica having an average particle size of about 0.05 ⁇ m to 10 ⁇ m can be easily obtained by the method of reacting metallic silicon with oxygen.
• Crushed silica is fine particles that can be produced by crushing silica. It is characterized by its angular surface. In particular, it is desirable to employ a form that can be obtained by crushing the spherical silica described above.
• the crushing method is not particularly limited. Examples include bead mills, jet mills, ball mills, and vibrating ball mills.
• Abrasive grains can be surface treated.
• a method using a silane compound can be exemplified.
• the silane compound those having an epoxy group, a vinyl group, a phenylamino group, or the like can be exemplified, and those having an epoxy group are preferred.
• the amount of treatment with the silane compound is not particularly limited, examples thereof include 1% or more, 2% or more, 3% or more, 4% or more, and 5% or more based on the mass of the entire abrasive grain.
• a resin material is used for the binder.
• a polishing layer is formed by dispersing the aforementioned abrasive grains in this binder.
• All resin materials are crosslinked.
• "all crosslinked” means that the crosslinkable precursor contained in the resin material accounts for 98% or more (preferably 99% or more, more preferably substantially 100%) based on the mass of the entire resin material.
• An epoxy resin can be exemplified as a crosslinkable precursor.
• the component derived from the epoxy resin means only the part derived from the epoxy resin precursor in one molecular chain when the epoxy resin precursor and other precursor are copolymerized.
• the epoxy resin is not particularly limited. Bisphenol type (A type, F type, mixture of A type and F type, etc.), biphenyl type, etc. can be employed, and biphenyl type is preferred.
• a biphenyl-type epoxy resin is a resin obtained by reacting a precursor of an epoxy resin having a biphenyl skeleton.
• Biphenyl-type epoxy resin exhibits high heat resistance due to the rigidity of the biphenyl structure.
• the biphenyl structure has high linearity, and when cured, it has high plastic deformation ability.
• Halogen-substituted products, alkyl-substituted products, hydrogenated products, and the like can be used for the biphenyl skeleton of the biphenyl-type epoxy resin.
• the methyl-substituted compound is preferably used from the point of handleability.
• bisphenol-type epoxy resin precursors include ZX-1059 (Nippon Steel Chemical & Materials Co., Ltd.).
• epoxy resin precursors having a biphenyl skeleton include "jER (registered trademark)" YX4000H, YX4000, YL6616, YL6121H, YL6640, YL6677 (manufactured by Japan Epoxy Resin Co., Ltd.), NC3000 (Nippon Kayaku Co., Ltd.) and the like.
• a cured product consisting only of a biphenyl-type epoxy resin precursor can be used, or it can be used in combination with a bisphenol-type epoxy resin precursor (for example, bisphenol A).
• a compound represented by the following general formula can be exemplified as a precursor of the bisphenol type epoxy resin.
• Each of the four Rs in the general formula can be independently selected from alkyl groups such as methyl, hydrogen, and halogens such as chlorine, and it is particularly preferred that all of them are methyl groups.
• the curing agent for the epoxy resin is not particularly limited, but it is preferable to use a phenol-type curing agent.
• a curing catalyst can also be added.
• Commercially available curing agents include TD2131 (DIC Corporation) and MEH4500 (Meiwa Kasei Co., Ltd.).
• the binder has a pencil hardness of 3H or higher.
• the pencil hardness can be increased by increasing the curing time of the epoxy resin.
• the lower limit of the curing time can be 5 minutes, 8 minutes, 10 minutes, 11 minutes, 13 minutes, 14 minutes, 16 minutes, and 20 minutes.
• a film-like abrasive material for ferrules can be provided by adopting a film-like member as a supporting substrate and forming an abrasive layer composed of abrasive grains and a binder on the surface thereof. Further, as the supporting substrate, it is possible to adopt a suitable form other than a film form, and an abrasive material for ferrules having a desired form can be obtained by forming an abrasive layer composed of abrasive grains and a binder on the surface thereof. Obtainable. Furthermore, even without a support base material, a polishing material for ferrules can be constructed only by a combination of abrasive grains and a binder.
• the material that constitutes the supporting base material should have the necessary elasticity and strength and be able to hold the polishing layer.
• films made of polyesters such as polyethylene terephthalate (PET) and polybutylene terephthalate, polycarbonates, and the like are suitable.
• PET polyethylene terephthalate
• polybutylene terephthalate polycarbonates
• the thickness is not particularly limited, and may be, for example, about 25 to 150 ⁇ m.
• a buffer layer may be formed in advance on the surface of the supporting substrate depending on the purpose, such as improving the adhesiveness between the supporting substrate and the polishing layer and patterning the surface of the polishing layer.
• an easy-adhesion layer may be formed on the surface of the support substrate to serve as a buffer layer.
• the easy-adhesion layer can be formed by, for example, applying a buffer coating liquid made of epoxy resin, acrylic resin, polyester resin, or the like to the surface of the supporting substrate and drying.
• the buffer layer may be formed by subjecting the surface of the support substrate to heat treatment, corona treatment, plasma treatment, etc., and corona treatment is particularly preferred.
• the ferrule abrasive according to the present embodiment is produced by appropriately dispersing abrasive grains in a binder.
• Abrasive grains are dispersed by kneading them together with the resin material that constitutes the binder, or by mixing and dispersing them in precursors such as monomers and prepolymers before becoming resin materials, and then reacting the precursors to form resin materials.
• the abrasive grains are previously dispersed in an organic solvent and slurried, and then mixed and dispersed in the binder.
• the organic solvent used as the dispersion medium is desirably a solvent that dissolves the resin (or its precursor) constituting the binder or an organic solvent that can be mixed with the precursor itself.
• the resin material that makes up the binder is epoxy resin, and in order to harden the epoxy resin, it is common to harden it by heating it at a certain temperature for a certain period of time. As curing conditions, it is preferable to cure for as long a time as possible. As the lower limit of the curing time, 5 minutes, 8 minutes, 11 minutes and 14 minutes can be exemplified, and the lower limit of 14 minutes is particularly preferable.
• the lower limit of the curing temperature is preferably 110°C, more preferably 120°C, and even more preferably 130°C.
• the upper limit of the curing temperature is preferably 180°C, more preferably 170°C, and even more preferably 160°C. These upper and lower limits can be combined arbitrarily.
• a polishing layer can be formed on the surface of the support base material by applying a mixture of the precursor and abrasive grains to the surface of the support base material and then reacting the precursor.
• the method of obtaining the silica particles that constitute the abrasive grains is not particularly limited, but general methods such as a method of reacting metal silicon with oxygen, a method of melting silica with heat, and a sol-gel method can be used. In particular, it is desirable to combine the method of reacting metallic silicon with oxygen and the sol-gel method.
• the abrasive grains are composed of silica particles with a peak top (mode diameter) of 20 nm as small diameter particles and silica particles with a volume average particle diameter of 200 nm that do not substantially contain coarse particles of 3 ⁇ m or more. was mixed so as to be 70% on the basis of.
• the binder comprises a biphenyl-type epoxy resin (all Rs in the above chemical formula are methyl groups) as a precursor of the resin material, a trisphenolmethane derivative (manufactured by Meiwa Kasei Co., Ltd., MEH7500) as a curing agent, and triphenylphosphine as a curing catalyst. They were used by mixing at a mass ratio of 100:95:2.
• Abrasive grains and binder were mixed at a mass ratio of 93.5:6.5 to form a slurry.
• the resulting slurry was coated on the surface of a PET resin plate as a support substrate to a thickness of 75 ⁇ m and a thickness of 3 ⁇ m, and then cured at 140° C. for 5 minutes to form a polishing layer. did.
• the surface of the supporting base material was previously subjected to corona treatment.
• ⁇ Test Examples 2 and 3 Abrasives were produced in the same manner as in Sample 1, except that the thickness of the abrasive layer was changed to 5 ⁇ m (Test Example 2) and 8 ⁇ m (Test Example 3), and used as the abrasives of each test example.
• Test 1 Using the polishing material of Test Example 1 and a commercially available polishing material (NTT-AT, ADS-127), 50 terminals of an LC/PC connector (zirconia ferrule, glass fiber) were fixed to a jig, and Bulls was used as a polishing machine. -3000 was used for polishing. All the pads used for fixing the abrasive had a hardness of 80.
• Polishing is performed in 5 stages: (a) diamond abrasive (9 ⁇ m), rotation speed 130 rpm, 15 seconds, (b) diamond abrasive (30 ⁇ m), rotation speed 130 rpm, 10 seconds, (c) diamond abrasive ( 9 ⁇ m), rotation speed 130 rpm, 15 seconds, (d) diamond abrasive (1 ⁇ m), rotation speed 130 rpm, 25 seconds, (e) abrasive of each test example, rotation speed 130 rpm, 25 seconds.
• the end face shape of the LC/PC connector was three-dimensionally measured, and the height of the end face of the glass fiber was measured with the end face of the zirconia ferrule as a reference.
• the negative direction is the direction in which the end surface of the glass fiber is recessed with respect to the end surface of the zirconia ferrule.
• the scratches are preferably 50% or less.
• the return loss is preferably 57 dB or more. It is preferable that there is no peeling of the abrasive layer of the abrasive.
• the fiber height is in the range ⁇ 20 nm.
• Test 2 LC/PC connectors were polished in the same manner as in Test 1 using the abrasives of Test Examples 2 and 3. As a result, there was no significant difference from the abrasive material of Test Example 1 in terms of scratch generation, return loss, and fiber height. (Table 3).
• Test 3 LC/PC connectors were polished in the same manner as in Test 1 using the abrasives of Test Examples 4 to 6. As a result, there was no significant difference from the abrasive material of Test Example 1 in terms of scratch generation, return loss, and fiber height. (Table 4). Further, when the pencil hardness of Test Examples 1 and 4 to 6 was measured, it was 2H in Test Example 1, 2H in Test Example 4, 2H in Test Example 5, and 3H in Test Example 6.
• Test 4 The same test as Test 1 was performed on each of the abrasives of Test Examples 1 and 7 to 9. After that, when the peeling of the abrasive material of each test example was observed, it was found that the abrasive material of Test Examples 7 to 9 had less peeling than the abrasive material of Test Example 1 and was superior in durability.

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• Polishing Bodies And Polishing Tools (AREA)

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• 2022
  • 2022-03-31 WO PCT/JP2022/016792 patent/WO2022220161A1/ja not_active Ceased
  • 2022-03-31 CN CN202280027867.9A patent/CN117120575A/zh active Pending
  • 2022-03-31 JP JP2023514608A patent/JP7634654B2/ja active Active
• 2023
  • 2023-10-16 US US18/380,228 patent/US12338368B2/en active Active

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