JP2000354951A - Polishing unit - Google Patents

Abstract

PROBLEM TO BE SOLVED: To improve dispersibility of silica pulverized powder to heighten the polishing accuracy in a polishing unit obtained by coating a polishing layer containing an abrasive pulverized powder and binder on a support, by using silica pulverized powder of sedimentating type as abrasive material pulverized powder of a polishing layer and specifying the thickness of the support. SOLUTION: This polishing unit 1 is suitably used for polishing the end face of a connector ferrule 5 for an optical fiber, in which an optical fiber 7 made of glass material such as quartz glass or the like is inserted and fixed in the central part thereof. The polishing unit 1 has a support 2 made of polyester film 25 to 150 μm thick. A polishing layer 3 contacting silica pulverized powder (abrasive material) of sedimentating type, whose average particle size of the single particles or aggregate particles is 0.1-4 μm and whose oil absorption is 100-250 ml/100 g, and a binder (30-10 pts.wt. to 100 pts.wt. silica pulverized powder) is stacked 5-25 μm thick on the support 2 to form into a polishing sheet of a designated shape such as a disc-like shape or the like.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polishing body such as a polishing sheet and a polishing disk used for polishing an end face of an optical fiber connector ferrule.

[0002]

2. Description of the Related Art For example, the end face of an optical connector ferrule in which an optical fiber is inserted and fixed in a ferrule hole is conventionally polished using a polishing body or a polishing slurry. Sufficient results have not always been obtained with respect to transmission loss and the like.

In other words, the end face of the connector ferrule for optical fiber contains different materials including many ceramics such as glass material, alumina, and zirconia, and these must be uniformly cut to prevent optical transmission loss. In particular, it has been extremely difficult to maintain the smoothness between the ferrule surface and the optical fiber surface, and to obtain a low reflection characteristic by polishing so as not to cause a step between the ferrule surface and the optical fiber surface.

[0004] As an example of the polishing body, Japanese Patent Application Laid-Open No. H8-3
As disclosed in JP 36758, a coating liquid for a polishing layer in which colloidal silica particles having an average particle size of 0.01 to 0.1 μm are dispersed in a binder is applied on a support to form a polishing layer. Polished bodies have been proposed.

[0005] By the way, the production of the above-mentioned abrasive body is as follows.
It is performed by a coating liquid dispersion device, a coating device, and, if necessary, a calendering process, a heat treatment device, a slit device (cutting device), a winding device, and the like.

[0006]

However, in the above-mentioned polishing body of the prior art, the average particle size is 0.01 to 0.01.
Although 0.1 μm colloidal silica particles are dispersed in the polishing layer, they are disadvantageous in terms of productivity, cost, and the like.

When the abrasive fine powder made of alumina or the like other than silica has a high Mohs hardness, the end face of the optical fiber may be damaged or a step may be generated between the end face of the ferrule and the Mohs altitude is low. In such a case, there is a possibility that the return loss is increased without a smooth surface due to insufficient polishing power.

The present invention has been made in view of the above points, and an object of the present invention is to provide a polishing body and a method of manufacturing a polishing body suitable for polishing the end face of an optical fiber connector ferrule by improving the dispersibility of silica fine powder. Things.

[0009]

According to the present invention, there is provided a polishing body comprising a support, on which a polishing layer containing fine abrasive powder and a binder is coated, for polishing an end face of an optical fiber connector ferrule. The polishing body according to any one of claims 1 to 3, wherein sedimentable silica fine powder is used as the abrasive fine powder of the polishing layer, and the thickness of the support is 25 to 150 µm.

The fine silica powder has an average particle size of 0.1.
Those having an oil absorption of 100 to 250 ml / 100 g at 1 to 4 μm are preferred. This silica fine powder is a sedimentable type, and unlike a gel type silica powder, is a small silica fine powder having a specific surface area of 180 m ² / g or less according to the BET method, easily having an open aggregated structure, and having a binder and While the gel type silica has excellent dispersibility in solvents and the like, the specific surface area by the BET method is 300 m ² /
Since it has a dense aggregate structure as large as about g, colloidal silica is not used in the present invention. The silica fine powder preferably has an average particle size of 0.1 to 4 μm of single particles or fine particles aggregated.
４4 μm is preferred.

It is possible to polish the surface of the polishing layer while supplying a polishing liquid comprising water or a slurry (for example, a silica slurry). At this time, the average particle size of the abrasive contained in the slurry is set to the above-mentioned value. It is preferable that the average particle size is smaller than the average particle size of the fine silica powder in the polishing layer.
This polishing liquid preferably does not contain a base or an acid.

The dry thickness of the polishing layer is 5 to 25 μm.
m is preferred in terms of durability. The binder is preferably used in an amount of 30 to 100 parts by weight based on 100 parts by weight of the silica fine powder.

It is preferable that the coating liquid for forming the polishing layer is dispersed by using a sand grinder in order to obtain good dispersibility. At this time, it is preferable to use glass beads, ceramic beads, and steel beads having a diameter of 0.2 to 10 mmφ. In addition, it is preferable that the surface of the polishing layer is subjected to a calendering treatment in order to obtain a desired surface property. This calendering process is performed at a linear pressure of 50 to 400 kg / cm and a temperature of 4 kg / cm.
A temperature of 0 to 120 ° C. and a speed of 5 to 500 m / min is preferred.
The calender roll can be arbitrarily selected from a metal roll, a resin roll, and the like.

[0014]

According to the abrasive body of the present invention as described above, the sedimentable silica fine powder is used as the abrasive of the abrasive layer provided on the support having a thickness of 25 to 150 μm. The sedimentation type silica fine powder is excellent in dispersibility of the coating solution, without causing excessive aggregation and gelation of particles,
It is uniformly dispersed in the binder, and the production efficiency is improved and the polishing body can be obtained at low cost. The obtained polishing layer has a strong film quality and the polishing performance is improved when the end face of the optical fiber connector ferrule is polished. At the same time, grinding scratches on the end face of the optical fiber can be reduced.

That is, in the optical fiber connector ferrule of which the end surface is polished by the polishing body of the present invention, the optical fiber tip portion has a predetermined curved surface shape without causing scratches on the surface to be polished, and the optical fiber (quartz glass). ) And a ferrule (such as zirconia) are polished without any step between the polished surfaces, and the return loss in light transmission when joining the polished end surfaces is -40.
It can be reduced to dB or less, and further, since there is no step, the end face is hardly stained.

In particular, the precipitated silica fine powder has an average particle size of 0.1 to 4 μm and an oil absorption of 100 to 2 μm.
The use of 50 ml / 100 g improves the dispersibility and the surface properties of the polishing layer, and is suitable for finish polishing of the connector ferrule for optical fibers. Furthermore, those in which the coating liquid is dispersed by a sand grinder to obtain high dispersibility of the silica fine powder, and those in which the smoothness of the polishing layer surface is adjusted by calendering treatment, can obtain suitable finish polishing characteristics. .

In the polishing with the polishing body of the present invention, a polishing liquid with water or a slurry can be used if necessary, and a lubricating and cooling property can be obtained, and the polishing liquid does not contain a base and an acid. This facilitates waste liquid treatment. In particular,
When the average particle size of the abrasive contained in the slurry is smaller than that of the silica fine powder in the polishing layer, it is effective in that polishing scratches on the end face of the optical fiber and a step with the tip of the ferrule do not occur.

The dry thickness of the polishing layer is preferably 5 to 25 μm, the thickness of the support is preferably 25 to 150 μm, and the thickness of the polishing layer is 5 to 150 μm.
If less than 25 μm, the durability at the time of polishing is insufficient.
A thickness exceeding 25 μm is practically unnecessary. If the thickness of the support is less than 25 μm, the support is thin and wrinkled, so that the polishing aptitude deteriorates.
If the thickness is too large, it will be difficult to handle the coating liquid at the time of coating, and it will be difficult to flatly attach the coating liquid to the substrate.

[0019]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, embodiments of a polishing body and a method for manufacturing the same according to the present invention will be described, and the present invention will be described in more detail. FIG. 1 shows a conceptual diagram of a state of polishing by a polishing body according to one embodiment.

The abrasive body 1 has a mean particle size of single particles or aggregated particles of 0.1 to 4 μm (or 1 to 4 μm) on a support 2 having a thickness of 25 to 150 μm made of a polyester film or the like, and an oil absorption amount. A polishing layer 3 containing sedimentable silica fine powder (abrasive) of 100 to 250 ml / 100 g and a binder (30 to 100 parts by weight with respect to 100 parts by weight of silica fine powder) is laminated to a thickness of 5 to 25 μm. It is formed on a polishing sheet having a predetermined shape such as a disk shape.

Optical fiber connector ferrule 5
Is a ferrule 6 made of ceramic material such as zirconia
The optical fiber 7 made of a glass material such as quartz glass is inserted and fixed in the center hole of the optical fiber. The tip of the connector ferrule 5 is polished by sticking the abrasive body 1 to an elastic body 11 such as rubber provided on a base 10 (turntable), and applying the tip of the connector ferrule 5 to the abrasive body 1 at a predetermined pressure. The base 10 or the connector ferrule 5 is made to relatively rotate in a planetary manner while the base 10 is rotated at a predetermined number of revolutions by pressing and contacting, and water or slurry (silica slurry) is supplied from the supply nozzle 15 to the polishing portion.
The polishing liquid 16 (coolant liquid) is supplied to perform wet polishing.

The polishing liquid 16 provides lubricating and cooling properties of the polished portion, and does not contain a base or an acid. When a silica slurry is used, the polishing slurry 16 is made of the same material as that of the silica of the polishing layer and the silica contained in the slurry. The average particle size is, for example, 0.005 to 0.1 μm, which is smaller than the average particle size of the fine silica powder of the polishing layer 3.

The relative movement of the base 10 and the connector ferrule 5 in polishing may be such that only one of them is moved, and the type of movement may be changed as appropriate.

Although the basic manufacturing process of the polishing body 1 is not shown, a coating liquid manufacturing apparatus (sand grinder) disperses and adjusts the above-mentioned polishing layer coating liquid containing the silica fine powder, binder, solvent and the like. This coating solution is applied to a predetermined thickness on a support running at a predetermined speed by a coating device, dried by a drying device to form a polishing layer, and thereafter, a calender device provided with a metal roll or a resin roll. The surface of the polishing layer is calendered, and if necessary, treated with a heat treatment device.
Then, it is formed into a predetermined shape by a punching process, a cutting process, or the like to form a polishing body. The center line average surface roughness Ra of the polishing layer surface of the obtained polishing body was 0.001.
５5 μm.

The particle size is measured, for example, using a Coulter counter (aperture 50 μm, D50
Diameter) and the oil absorption is JISK5101, 21
by.

As the abrasive fine powder used in the polishing layer of the present invention, the above-mentioned sedimentation type silica fine powder is used alone or together with another abrasive. Other abrasives have a Mohs hardness of 6 to 10 and include 30% or less of the total amount of powder. The abrasive is generally a material having an abrasive action or a polishing action, such as α-alumina, γ-alumina, α, γ-alumina, fused alumina, silicon carbide, chromium oxide, corundum, artificial diamond, diamond, α -Iron oxide, silicon nitride, boron nitride, molybdenum carbide, boron carbide, tungsten carbide, titanium carbide, zirconia, titanium oxide, cerium oxide, red iron oxide, garnet, etc., and up to 4 types of materials with a Mohs hardness of 7 or more Can be used in combination. These abrasives have an average particle size of 0.
Those having a size of 1 to 25 μm are used. Specific examples of the abrasive include AKP1, AKP15, and Sumitomo Chemical Co., Ltd.
AKP20, AKP30, AKP50, AKP80, H
It50, Hit100, and the like. These are described in JP-B-52-28642 and JP-B-49-394.
02, JP-A-63-98828, U.S. Pat.
No. 725, U.S. Pat. No. 3,077,807, U.S. Pat.
No. 1196, U.S. Pat. No. 3,293,066, U.S. Pat.
No. 30910, U.S. Pat. No. 3,833,412, U.S. Pat.
No. 117190, British Patent 1145349, West German Patent 853211 and the like.

As the binder used in the polishing layer of the present invention, conventionally known thermoplastic resins, thermosetting resins, reactive resins, electron beam curing resins, ultraviolet ray curing resins, visible ray curing resins, and the like. Is used.

As the thermoplastic resin, the softening temperature is 200
C. or lower, having an average molecular weight of 10,000 to 300,000 and a degree of polymerization of about 50 to 2,000, more preferably 20 to 2,000.
It is about 0 to 800. For example, vinyl chloride vinyl acetate copolymer, vinyl chloride copolymer, vinyl chloride vinyl acetate vinyl alcohol copolymer, vinyl chloride vinyl alcohol copolymer, vinyl chloride vinylidene copolymer, vinyl acrylonitrile copolymer, acrylic acid Ester acrylonitrile copolymer, acrylate vinylidene chloride copolymer, acrylate styrene copolymer, methacrylate acrylonitrile copolymer,
Methacrylic acid ester vinylidene chloride copolymer, methacrylic acid ester styrene copolymer, urethane elastomer, nylon-silicone resin, nitrocellulose-polyamide resin, polyfucca vinyl, vinylidene chloride acrylonitrile copolymer, butadiene acrylonitrile copolymer, polyamide Resins, polyvinyl butyral, cellulose derivatives (cellulose acetate butyrate, cellulose diacetate, cellulose triacetate, cellulose propionate, nitrocellulose, ethyl cellulose, methyl cellulose, propyl cellulose, methyl ethyl cellulose, carboxymethyl cellulose,
Acetylcellulose), various synthetic rubber-based thermoplastic resins such as styrene-butadiene copolymer, polyester resin, polycarbonate resin, chlorovinyl ether acrylate copolymer, amino resin, polyamide resin, and mixtures thereof. .

Examples of these resins are described in JP-B-37-68.
No. 77, JP-B-39-12528, JP-B-39-19
No. 282, No. 40-5349, No. 40-20
No. 907, JP-B-41-9463, JP-B-41-14
No. 059, JP-B-41-16985, JP-B-42-6
No. 428, JP-B-42-11621, JP-B-43-4
No. 623, JP-B-43-15206, JP-B-44-2
No. 889, No. 44-17947, No. 44-1
No. 8232, No. 45-14020, No. 45-
14500, JP-B-47-18573, JP-B-47
-22063, JP-B-47-2264, JP-B-4
7-22068, JP-B-47-22069, JP-B-47-22070, JP-B-47-27886, JP-A-57-133521, JP-A-58-137133.
JP-A-58-166533, JP-A-58-222
No. 433, JP-A-59-58642 and the like.
No. 71364, U.S. Pat. No. 4,752,530, and the like.

The thermosetting resin or the reactive resin has a molecular weight of 200,000 or less in the state of a coating liquid, and becomes infinite by a reaction such as condensation and addition by heating and humidifying after coating and drying. Is preferred. Among these resins, those which do not soften or melt before the resin is thermally decomposed are preferable. Specifically, for example, a phenol resin, a phenoxy resin, an epoxy resin, a polyurethane resin, a polyester resin, a polyurethane polycarbonate resin, a urea resin, a melamine resin, an alkyd resin, a silicone resin, an acrylic reaction resin (an electron beam curing resin), and an epoxy-polyamide Resin, nitrocellulose melamine resin, mixture of high molecular weight polyester resin and isocyanate prepolymer, mixture of methacrylate copolymer and diisocyanate prepolymer, mixture of polyester polyol and polyisocyanate, urea formaldehyde resin, low molecular weight glycol / high molecular weight A diol / triphenylmethane triisocyanate mixture, a polyamine resin, a polyimine resin, and mixtures thereof.

Examples of these resins are described in JP-B-39-810.
No. 3, JP-B-40-9779, JP-B-41-7192
No., JP-B-41-8016, JP-B-41-14275
No., JP-B-42-18179, JP-B-43-1208
No. 1, Japanese Patent Publication No. 44-28023, Japanese Patent Publication No. 45-145
No. 01, JP-B-45-24902, JP-B-46-13
103, JP-B-47-2265, JP-B-47-2
No. 2066, JP-B-47-22067, JP-B-47-
22072, JP-B-47-22073, JP-B-47
-28045, JP-B-47-28048, JP-B-4
It is described in publications such as 7-28922.

These thermoplastic resins, thermosetting resins and reactive resins have a functional group other than the main functional group, such as carboxylic acid (COOM), sulfinic acid, sulfenic acid, sulfonic acid (SO ₃ M) and phosphoric acid (PO ₃ M). (OM) (OM)), phosphonic acid, sulfuric acid (OSO ₃ M), and acidic groups such as ester groups thereof (M is H, an alkali metal, an alkaline earth metal,
Hydrocarbon groups), amino acids; aminosulfonic acids, sulfuric acid or phosphoric acid esters of amino alcohols, amphoteric groups such as alkyl betaine, amino groups, imino groups, imide groups,
An amide group, etc., a hydroxyl group, an alkoxyl group, a thiol group, an alkylthio group, a halogen group (F, Cl, Br,
I) a silyl group, a siloxane group, an epoxy group, an isocyanato group, a cyano group, a nitrile group, an oxo group, an acryl group, and a phosphine group. ^-6 eq ~ 1 × 10 ^-2
It is preferable to include eq.

The polyisocyanate as a curing agent used in the polishing layer of the present invention includes tolylene diisocyanate, 4,4'-diphenylmethane diisocyanate, hexamethylene diisocyanate, xylylene diisocyanate, naphthylene-1,5-diisocyanate, o-
Isocyanates such as toluidine diisocyanate, isophorone diisocyanate, triphenylmethane triisocyanate, isophorone diisocyanate, products of the isocyanates and polyalcohols, polyisocyanates of 2 to 10-mers produced by condensation of isocyanates, polyisocyanates and polyurethanes And those whose terminal functional groups are isocyanates can be used. The average molecular weight of these polyisocyanates is preferably 100 to 20,000.

Commercially available trade names of these polyisocyanates include Coronate L, Coronate HL, Coronate 2030, Coronate 2031, Millionate MR, Millionate MTL (manufactured by Nippon Polyurethane Co., Ltd.), Takenate D-102, and Takenate D-110.
N, Takenate D-200, Takenate D-202, Takenate 300S, Takenate 500 (manufactured by Takeda Pharmaceutical Co., Ltd.), Sumidur T-80, Sumidur 44S, Sumidur PF, Sumidur L, Sumidur N, Desmodur L , Death module IL, death module N, death module HL, death module T65, death module 15, death module R, death module R
F, death module SL, death module Z4273
(Manufactured by Sumitomo Bayer Co., Ltd.), and these can be used alone or in combination of two or more by utilizing the difference in curing reactivity.

For the purpose of accelerating the curing reaction, a hydroxyl group (butanediol, hexanediol, having a molecular weight of 100
A compound having an amino group (such as monomethylamine, dimethylamine, or trimethylamine), a metal oxide catalyst, or a catalyst such as iron acetylacetonate can also be used in combination. It is desirable that these compounds having a hydroxyl group or an amino group are polyfunctional. These polyisocyanates have a total amount of binder resin and polyisocyanate of 10 in the polishing layer and the back layer.
It is preferably used in an amount of 2 to 70 parts by weight per 0 parts by weight, more preferably 5 to 50 parts by weight. Examples of these are disclosed in JP-A-60-131622 and JP-A-61-741.
No. 38 and the like.

In addition, compounds having various functions are added to the polishing layer as additives. For example, a dispersant, a lubricant, an antistatic agent, an antioxidant, a fungicide, a coloring agent, a solvent, and the like are added.

The powdery lubricant used in the present invention includes graphite, molybdenum disulfide, boron nitride, graphite fluoride, calcium carbonate, barium sulfate, silicon oxide, titanium oxide, zinc oxide, tin oxide, and tungsten disulfide. Inorganic fine powder, acrylic styrene resin fine powder, benzoguanamine resin fine powder, melamine resin fine powder, polyolefin resin fine powder, polyester resin fine powder, polyamide resin fine powder, polyimide resin fine powder, polyimide resin fine powder There are resin fine powders such as ethylene resin fine powder.

As the organic compound-based lubricant, silicone oil (dialkyl polysiloxane, dialkoxy polysiloxane, phenyl polysiloxane, fluoroalkyl polysiloxane (KF96, KF69 manufactured by Shin-Etsu Chemical Co., Ltd.)
)), Fatty acid-modified silicone oil, fluoroalcohol, polyolefin (polyethylene wax, polypropylene, etc.), polyglycol (ethylene glycol, polyethylene oxide wax, etc.), tetrafluoroethylene oxide wax, polytetrafluoroglycol, perfluoroalkyl ether, perfluoro Fatty acids, perfluoro fatty acid esters, perfluoroalkyl sulfates, perfluoroalkyl sulfonates, perfluoroalkylbenzene sulfonates, perfluoroalkyl phosphates, and other compounds containing fluorine or silicon, alkyl sulfates, alkyl sulfonates , Alkyl phosphonic acid triester,
Organic acids and organic acid ester compounds such as alkyl phosphonic acid monoesters, alkyl phosphonic acid diesters, alkyl phosphates, succinates, etc., triazaindolizine, tetraazaindene, benzotriazole, benzotriazine, benzodiazole, EDTA, etc. nitrogen·
Heterocyclic compound containing sulfur, having 10 to 40 carbon atoms
Consisting of a monobasic fatty acid of formula (I) and any one or more of monohydric or dihydric alcohols having 2 to 40 carbon atoms, trihydric alcohol, tetrahydric alcohol, and hexahydric alcohol Esters, fatty acid esters of monohydric to hexavalent alcohols having a total of 11 to 70 carbon atoms in total with monobasic fatty acids having 10 or more carbon atoms and carbon atoms of the fatty acids, 8 to 40 carbon atoms And fatty acid amides, fatty acid alkyl amides and aliphatic alcohols.

Specific examples of these compounds include butyl caprylate, octyl caprylate, ethyl laurate, butyl laurate, octyl laurate, ethyl myristate, butyl myristate, octyl myristate, 2-ethylhexyl myristate, Ethyl palmitate, butyl palmitate, octyl palmitate, 2 ethylhexyl palmitate, ethyl stearate, butyl stearate, isobutyl stearate, octyl stearate, 2 ethylhexyl stearate, amyl stearate, isoamyl stearate, 2 stearic acid
Ethylpentyl, 2-hexyldecyl stearate, isotridecyl stearate, stearic acid amide, alkyl stearate, butoxyethyl stearate,
Anhydrosorbitan monostearate, anhydrosorbitan distearate, anhydrosorbitan tristearate, anhydrosorbitan tetrastearate, oleyl oleate, oleyl alcohol, lauryl alcohol, montan wax, carnauba wax, etc. used alone or in combination it can.

The lubricant used in the present invention includes:
Lubricating oil additives can be used alone or in combination. Antioxidants known as rust inhibitors (metal chelates such as alkylphenol, benzotriazine, tetraazaindene, sulfamide, guanidine, nucleic acid, pyridine, amine, hydroquinone, EDTA, etc.) Agents), rust inhibitors (naphthenic acid, alkenyl succinic acid, phosphoric acid, dilauryl phosphate, etc.), oil agents (rapeseed oil, lauryl alcohol, etc.), extreme pressure agents (dibenzyl sulfide, tricresyl phosphate, tributyl) Phosphite, etc.), detergents / dispersants, viscosity index improvers, pour point depressants, foaming agents and the like. These lubricants are added in the range of 0.01 to 30 parts by weight based on 100 parts by weight of the binder. These are described in JP-B-43-23889 and JP-B-48-24.
No. 041, JP-B-48-18482, JP-B-44-1
No. 8221, JP-B-47-28043, JP-B-57-
No. 56132, JP-A-59-8136, JP-A-59-8136
No. 8139, JP-A-61-85621, U.S. Pat.
No. 23233, US Pat. No. 3470021, US Pat.
492,235, U.S. Pat. No. 3,497,411, U.S. Pat.
US Patent No. 4,552,794, IBM Technical
Disclosure Bulletin (IBM Technica
l Disclosure Bulletin) Vo
l. 9, No7, p779 (December 1966), Electronic (ELEKTRONIK) 1961 No1
2, p380, Handbook of Chemistry, Application, p954-967,
It is described in the publication of Maruzen shares in 1980.

Examples of the dispersing agent and dispersing agent for the abrasive used in the present invention include caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, elaidic acid, linoleic acid, linolenic acid, C2 of stearic acid, behenic acid, maleic acid, phthalic acid, etc.
40 pieces of fatty acids (R ₁ COOH, R ₁ is carbon 1-39
Alkyl groups, phenyl groups, aralkyl groups), alkali metals (Li, Na, K, NH ₄ ^+, etc.) or alkaline earth metals (Mg, Ca, Ba, etc.) of the above fatty acids, Cu, P
Metallic soaps (copper oleate), fatty acid amides, lecithin (soybean oil lecithin) and the like comprising b. In addition, higher alcohols having 4 to 40 carbon atoms (butanol, octyl alcohol, myristyl alcohol, stearyl alcohol) and their sulfates, sulfonic acids,
Phenylsulfonic acid, alkylsulfonic acid, sulfonic acid ester, phosphoric acid monoester, phosphoric diester, phosphoric triester, alkylphosphonic acid, phenylphosphonic acid, amine compounds and the like can also be used. In addition, polyethylene glycol, polyethylene oxide, sulfosuccinic acid, metal salts of sulfosuccinic acid, sulfosuccinate, and the like can also be used. One or more of these dispersants are usually used, and one kind of the dispersant is added in an amount of 0.005 to 20 parts by weight based on 100 parts by weight of the binder. Regarding the method of using these dispersants, the dispersants may be pre-applied to the surface of the abrasive or the non-abrasive fine powder, or may be added during dispersion.
Such a thing is, for example, JP-B-39-28369,
JP-B-44-17945, JP-B-44-18221
No., JP-B-48-7441, JP-B-48-15001
No., JP-B-48-15002, JP-B-48-1636
No. 3, JP-B-49-39402, U.S. Pat.
No. 93 and No. 3470021.

The fungicides used in the present invention include 2- (4
-Thiazolyl) -benzimidazole, N- (fluorodichloromethylthio) -phthalimide, 10.10'-
Oxybisphenoxalcin, 2,4,5.6 tetrachloroisophthalonitrile, P-tolyldiiodomethylsulfone, triiodoallyl alcohol, dihydroacetoacid, mercury phenyloleate, bis (tributyltin) oxide, saltylani There are rides. Such a substance is described in, for example, "Microbial Disaster and Prevention Technology", Engineering Book, 1972, "Chemistry and Industry", 32, 904 (1979).

As the antistatic agent used in the present invention, carbon black can be used.
Thermal for rubber, black for color, acetylene black and the like can be used. Its specific surface area is 5-500
m ² / g, DBP oil absorption 10-400 ml / 100
g, pH 2-10, water content 0.1-10%, tap density 0.1-1 g / cm ² . As a specific example of this carbon black, BLACKPEARLS 2000, 1300, 1 manufactured by Cabot Corporation
000,900,800,700, manufactured by Mitsubishi Chemical Corporation:
650B, 950B, 3250B, 850, 900, 9
60,980,1000,2300,2400,260
0 and the like. In addition, carbon black that has been subjected to surface treatment with a dispersant or the like or graphitized with a resin can also be used.

As the antistatic agent other than carbon black used in the present invention, graphite, modified graphite,
Conductive powders such as carbon black graft polymer, tin oxide-antimony oxide, tin oxide, titanium oxide-tin oxide-antimony oxide; natural surfactants such as saponin; alkylene oxide-based, glycerin-based, glycidol-based, polyhydric alcohol, Nonionic surfactants such as polyhydric alcohol esters and alkylphenol EO adducts; higher alkylamines, cyclic amines, hydantoin derivatives, amidoamines, esteramides, quaternary ammonium salts, pyridine and other heterocycles, phosphoniums and sulfoniums Anionic surfactants containing acidic groups such as carboxylic acid, sulfonic acid, phosphonic acid, phosphoric acid, sulfate ester group, phosphonate ester, phosphate ester group; amino acids; aminosulfonic acids, sulfuric acid of amino alcohol or Phosphoric esters, amphoteric surfactants such as alkyl betaine type and the like are used.

Some of the examples of the surfactant compound which can be used as the antistatic agent are described in JP-A-60-28025, US Pat. Nos. 2,271,623, 2,224,472, and 22.
88226, 2676122, 2676924
Nos. 2,676,975, 2,691,566,27
27860, 2730498, 2742379
Nos. 2739891, 3068101, 31
No. 58484, No. 3201253, No. 32010191
Nos. 3,294,540, 3,415,649 and 34
No. 41413, No. 3444254, No. 3475174
No. 3,545,974, West German Patent Publication (OLS) 19
No. 42665, British Patent Nos. 1077317 and 1198
No. 450, Ryohei Oda et al., "Synthesis of Surfactants and Their Applications" (Maki Shoten, 1972 edition); W. "Surfes Active Age Entities" by Beili (Interscience Publication Corporation 1
985); P. Encyclopedia of Surfactive Agents, Vol. 2 (Chemical publishing company, 1964 edition) by Sisley; Surfactant Handbook, 6th printing (Sangyo Tosho Co., Ltd.,
December 20, 1966); Hideo Marumo, "Antistatic Agent"
Koshobo (1968) and the like.

These surfactants may be added alone or as a mixture. The amount of these surfactants used in the abrasive body is 0.01 to 10 parts by weight per 100 parts by weight of the abrasive. The amount used in the back layer is 10 binders.
It is 0.01 to 30 parts by weight per 0 parts by weight. These are used as antistatic agents, but are sometimes applied for other purposes such as improvement of dispersion, improvement of lubricity, coating aid, wetting agent, curing accelerator, and dispersion accelerator. .

As the organic solvent used in the dispersion, kneading and coating of the present invention, ketones such as acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, isophorone and tetrahydrofuran in any ratio; methanol, ethanol, propanol and butanol , Isobutyl alcohol, isopropyl alcohol, alcohols such as methylcyclohexanol; methyl acetate,
Ester systems such as ethyl acetate, butyl acetate, isobutyl acetate, isopropyl acetate, ethyl lactate and glycol monoethyl ether; ether systems such as diethyl ether, tetrahydrofuran, glycol dimethyl ether, glycol monoethyl ether and dioxane; benzene, toluene, xylene, Tar-based (aromatic hydrocarbons) such as cresol, chlorobenzene, and styrene; chlorinated hydrocarbons such as methylene chloride, ethylene chloride, carbon tetrachloride, chloroform, ethylene chlorohydrin, and dichlorobenzene; NN-dimethylformaldehyde , Hexane and the like can be used. These solvents are generally used in two or more kinds at an arbitrary ratio. Further, a trace amount of impurities (polymer of the solvent itself, moisture, raw material components, etc.) may be contained in an amount of 1% by weight or less.

The polishing layer is formed by dissolving the above composition and the like in a solvent by arbitrarily combining the above-mentioned compositions and the like, coating the solution on a support as a coating solution.
dry. As the material of the support, polyethylene terephthalate, polyesters such as polyethylene naphthalate, polyolefins such as polypropylene, cellulose derivatives such as cellulose triacetate and cellulose diacetate, vinyl resins such as polyvinyl chloride,
In addition to plastics such as polycarbonate, polyimide, polyamide, and polysulfone, metals such as aluminum and copper, and ceramics such as glass can also be used. Prior to coating, these supports may be subjected to corona discharge treatment, plasma treatment, undercoating treatment, heat treatment, dust removal treatment, metal deposition treatment, and alkali treatment. For these supports,
For example, West German Patent 3338854A, Japanese Patent Laid-Open No. 59-116
No. 926, JP-A-61-129731, U.S. Pat.
No. 88368; Yukio Mitsuishi, Textile and Industry, vol. 31, p5
0-55, 1975, and the like. The center line average surface roughness of these supports is 0.001 to 0.5 μm
(Cutoff value 0.25 mm) is preferred. In addition, the Young's modulus (F5 value) of these supports is determined in the width direction,
100 to 1000 kg / mm ² (1 kg / mm)
m ² = 9.8 Pa) can be selected.

The method of dispersion and kneading is not particularly limited, and the order of addition of each component (resin, powder, lubricant, solvent, etc.),
The addition position during dispersion / kneading, the dispersion temperature (0 to 80 ° C.) and the like can be appropriately set. A sand grinder disperser is preferably used for the preparation of the polishing paint, but other kneaders such as a two-roll mill, a three-roll mill, a ball mill, a pebble mill, a tron mill, a Segvari attritor, and a high-speed impeller may be used. ,
Disperser, high-speed stone mill, high-speed impact mill, disper, kneader, high-speed mixer, ribbon blender, co-kneader, intensive mixer, tumbler, blender, disperser, homogenizer, single screw extruder, twin screw extruder, and super A sound disperser or the like can be used. Usually, a plurality of these dispersing and kneading machines are provided for dispersing and kneading, and the treatment is continuously performed.
For details of the technique relating to kneading and dispersion, see T.A. C. PATTON
Written by T.C. Patton, "Paint Flow"
and Pigment Dispersion "(Paint Flow and Pigment Dispersion), published in 1964 by John Wiley & Sons (John Wiley and Sons), Shinichi Tanaka, Industrial Materials, Vol. 25, 37 (1977), and references cited in the book. As an auxiliary material for the dispersion and kneading, a steel ball, a steel bead, a ceramic bead, a glass bead, and an organic polymer bead having an equivalent sphere diameter of 10 cmφ to 0.05 mmφ are used in order to efficiently promote the dispersion and kneading. These materials are not limited to spherical shapes, and U.S. Pat.
Nos. 414 and 2855156 are also described. Also in the present invention, a polishing layer coating liquid can be prepared by kneading and dispersing according to the method described in the above book or the cited document of the book.

As a method of applying the above-mentioned coating liquid for a polishing layer on a support, the viscosity of the coating liquid is adjusted to 1 to 20,000 centistokes (25 ° C.), and an air doctor coater, a blade coater, an air knife coater, a squeeze Coater, impregnated coater, reverse roll coater, transfer roll coater, gravure coater, kiss coater, cast coater, spray coater, rod coater, forward rotation roll coater, curtain coater, extrusion coater, bar coater, lip coater, etc. can be used, and other methods It is also possible to provide specific descriptions of these in “Coating Engineering” published by Asakura Shoten, pages 253 to 2
This is described in detail on page 77 (issued in 1963, 1963). When the polishing layer has a multilayer structure, simultaneous multilayer coating, sequential multilayer coating, or the like may be performed. These are described, for example, in JP-A-57-123532 and JP-B-62-2.
No. 37451, JP-A-59-142741,
This is disclosed in the specification of JP-A-59-165239.

The coating liquid applied to the support by such a method is dried in multiple stages at 20 ° C. (room temperature) to 130 ° C., and the formed polishing layer is dried to a thickness of about 5 to 15 μm. . Then, calendering is performed to adjust the surface roughness of the surface of the polishing layer formed as described above to enhance smoothness. Preferably, at least one of the calender rolls in the calendering process is a metal roll, and the metal roll is pressurized in contact with the polishing layer surface. In addition, a heat-resistant plastic roll such as epoxy, polyimide, polyamide, or polyimide amide can be used for the calender roll, and the treatment can be performed between metal rolls. The processing temperature is preferably 40
~ 120 ° C, linear pressure is preferably 50 ~ 400Kg / cm,
The speed is between 5 and 500 m / min.

The production method as described above is used for the preliminary treatment of powder.
It is desirable that the steps of surface treatment, kneading / dispersing, coating / drying, smoothing treatment, heat treatment, EB treatment, ultraviolet curing treatment, surface polishing treatment, and winding up be performed continuously. These are described, for example, in Japanese Patent Publication No. 40-23625 and Japanese Patent Publication No. 39-2.
No. 8368, Japanese Patent Publication No. 47-38802, British Patent No. 1191424, Japanese Patent Publication No. 48-11336, JP-A-49-53631, JP-A-50-1120.
No. 05, JP-A-51-77303, JP-B-52-17
No. 404, JP-A-60-70532, JP-A-2-
No. 2,656,672, U.S. Pat. No. 3,473,960, U.S. Pat. No. 4,728,569, U.S. Pat. No. 4,746,542, and the like. The method disclosed in Japanese Patent Publication No. 41-13181 is considered to be a basic and important technique in this field.

The wound abrasive body is formed into an abrasive body such as an abrasive sheet having a predetermined shape by punching, cutting or the like.
It is desirable to burnish and / or clean the abrasive body before or after performing these processes. Burnish polished body, specifically sapphire blade, razor blade,
Using a hard material such as a carbide material blade, diamond blade, or ceramic blade, the protruding portion of the polished surface is smoothed. The Mohs hardness of these materials is preferably 8 or more, but is not particularly limited as long as protrusions can be removed. The shape of these materials does not need to be a blade in particular, and shapes such as a square shape, a round shape, and a wheel (these materials may be provided around a rotating cylindrical shape) can be used. Cleaning of the abrasive body is performed by wiping the surface layer with a nonwoven fabric or the like for the purpose of removing surface dirt and excess lubricant. Such wiping materials include, for example, various types of Vilene manufactured by Japan Vilene Co., Ltd., Toraysee, Ecseine manufactured by Toray Industries, Kimwipe, various types of abrasives manufactured by Fuji Photo Film Co., Ltd. Tissue paper, such as nonwoven fabric made of rayon, nonwoven fabric made of acrylonitrile, and blended nonwoven fabric can be used. These are described, for example, in JP-B-46-39309.
No., JP-B-58-46768, JP-A-56-9042.
9, JP-B-58-46767, JP-A-63-259
No. 830, JP-A-1-201824 and the like.

The abrasive used in the present invention, the binder,
Additives (lubricants, dispersants, antistatic agents, surface treatment agents, carbon black, abrasives, light-blocking agents, antioxidants, antifungal agents, etc.), solvents and supports (undercoat layer, back layer, under back) (It may have a coating layer) or the production method thereof can be referred to the production method described in JP-B-56-26890 or the like.

[0055]

EXAMPLES Examples and comparative examples of the present invention will be shown below.
Evaluate its properties. In the examples, "parts" indicates "parts by weight".

<Examples 1 to 3> A binder and a solvent excluding isocyanate were mixed with 100 parts of the fine silica powder in the following coating liquid composition for a polishing layer, and the resulting dispersion was weighed to a size of 0.25 gallon. Place in a sand grinder, add 700g of 1.2mmφ glass beads, add 170g
Run at 0 rpm for 150 minutes to evenly disperse.
Thereafter, the number of revolutions is reduced to 500 rpm, the viscosity is adjusted, and a coating liquid for a polishing layer mixed with isocyanate (curing agent) is prepared. This coating solution is applied on a support made of a 75 μm-thick polyester film (PET) by a blade coater and then dried, and the dried coating film has a thickness of 12 μm.
Thus, a polished body on which a polishing layer of m was formed was obtained. This abrasive body was punched into a disk shape to obtain a sample as an abrasive sheet.

Examples 1 to 3 differ in the size of the abrasive and oil absorption. In Example 1, sedimentable silica fine powder having an average particle size of 1.5 μm (oil absorption 130 ml / 100 g).
Example 2 has an average particle size of 2.5 μm (oil absorption 110
Example 3 uses a sedimentable silica fine powder having an average particle size of 4 μm (oil absorption 200 ml / 100 g). The center line average surface roughness Ra of the polishing layer surface in the polishing body of Example 2 was 0.1 μm.

The polishing bodies of Examples 1 to 3 were attached on the elastic body of the base, and a polishing test of the connector ferrule was performed. In this polishing test, the above-mentioned base is made to rotate in a planetary manner, and the rotation is 24 rpm and the revolution is 2 rpm.
Twelve connector ferrules were attached to a jig, and the tip surface was pressed against the surface of the polishing layer at a rate of 20 g / piece (total load 240 g) to perform polishing for 30 seconds. 1 cc of water (or slurry) was dropped on the polishing layer as a polishing liquid.

Table 1 shows the presence / absence of scratches on the optical fiber surface by the above-mentioned polishing test (no scratches: 、, scratches: x), and the measurement results of the return loss of the optical fiber end surface after polishing.

The return loss (dB) is a value obtained by measuring the loss of the amount of transmitted light caused by the reflection of the polished surface of the optical fiber, and can evaluate the smoothness of the surface.
The output light amount is represented by -10 log (P1 / P2) when the output light amount is P1, and the greater the dB value is in the negative direction, the lower the reflection, the smaller the transmission loss, and the better the transmission state.

<Comparative Examples 1 and 2> Table 1 also shows the results of similar polishing tests performed on the polished bodies of Comparative Examples 1 and 2. In Comparative Example 1, the material of the abrasive was alumina (# 80).
00) and an average particle size of 1.5 μm (oil absorption 5 ml / 10
0g). In Comparative Example 1, the coating composition was the same as in Examples 1 to 3 except for the abrasive.

Comparative Example 2 is an example using colloidal silica (average particle size: 0.01 to 0.015 μm) as an abrasive. The composition of the coating liquid is as follows: polymer silicone resin (HPC-7502): 30%, 20 parts Colloidal silica: 30%, 80 parts The coating liquid is dispersed by ultrasonic dispersion, and the thickness is 75 μm.
m on a support made of a polyester film (PET) to form a polishing layer with a dry thickness of 3 μm.

From the results shown in Table 1, in Examples 1 to 3 of the present invention, good results were obtained with respect to both the damage on the fiber surface and the return loss. On the other hand, in the case of the fine powder of alumina of Comparative Example 1, the fiber surface after polishing was damaged, and the return loss was large. In the case of the colloidal silica of Comparative Example 2, there was no damage on the fiber surface, but the return loss was lower than that of the example of the present invention.

[Coating Composition for Polishing Layer] Abrasive (material: X, average particle size: Y) 100 parts Binder (vinyl chloride resin, 400X110A: manufactured by Zeon Corporation) 10 parts Binder (sulfonate group-containing polyurethane resin, UR8200: Toyobo Co., Ltd. 30 parts Binder (polyisocyanate, Coronate L: Nippon Polyurethane Co., Ltd.) 30 parts MEK (methyl ethyl ketone) / Anon 150 parts Butyl acetate 50 parts

[0065]

[Table 1]

[Brief description of the drawings]

FIG. 1 is a front view conceptually showing a polished state of an optical fiber connector ferrule by a polishing body according to one embodiment of the present invention.

[Explanation of symbols]

 REFERENCE SIGNS LIST 1 abrasive body 2 support 3 polishing layer 5 connector ferrule for optical fiber 6 ferrule 7 optical fiber 10 base 11 elastic body 15 supply nozzle 16 polishing liquid

 ──────────────────────────────────────────────────続 き Continued on the front page F-term (reference)

Claims (7)

[Claims] 1. A polishing body for polishing an end face of an optical fiber connector ferrule, comprising a support and a polishing layer containing fine abrasive powder and a binder coated thereon, wherein the fine polishing powder for the polishing layer is used. Using a sedimentation type silica fine powder, the thickness of the support is 25 to 150 μm
A polishing body, characterized in that: 2. The polishing body according to claim 1, wherein the silica fine powder has an average particle size of 0.1 to 4 μm and an oil absorption of 100 to 250 ml / 100 g. 3. The polishing body according to claim 1, wherein the polishing is performed in a state where a polishing liquid comprising water or slurry is supplied to the surface of the polishing layer. 4. The polishing body according to claim 3, wherein an average particle size of the abrasive contained in the slurry is smaller than an average particle size of the silica fine powder of the polishing layer. 5. The polishing body according to claim 1, wherein the dry thickness of the polishing layer is 5 to 25 μm. 6. The polishing body according to claim 1, wherein the coating liquid for coating the polishing layer is dispersed by using a sand grinder. 7. The polishing body according to claim 1, wherein a surface of the polishing layer is subjected to a calendering treatment.