JP2001009737A - Abrasive body - Google Patents

Abstract

PROBLEM TO BE SOLVED: To improve discursiveness of an abrasive, and to make the abrasive suitable for polishing an end surface of a connector ferrule for an optical fiber by using titanium oxide fine powder having the average particle size of a specific value as abrasive fine powder of an abrasive layer, and setting a thickness of a support to a specific value. SOLUTION: In an abrasive body 1, titanium oxide fine powder having the average particle size of 0.01 to 4 μm is used as an abrasive of an abrasive layer 3 arranged on a support 2 having a thickness of 25 to 150 μm. This titanium oxide fine powder has excellent dispersiveness in an applying liquid 16 to be uniformly dispersed in a binder without causing excessive coagulation and gelatinization of particles, production efficiency is improved, the abrasive body 1 can be inexpensively obtained, the obtained abrasive layer 3 becomes strong in a film quality, and has Moh's hardness equal to a silica particle. When polishing an end surface of a connector ferrule 5, polishing performance is improved, and a grinding flaw of an end surface of an optical fiber 7 can be reduced. Polishing can be performed without generating a step difference between abrasive surfaces of the optical fiber 7 and a ferrule 6.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

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

[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, such fine silica particles are difficult to disperse, and are disadvantageous in terms of productivity, cost, and the like.

[0007] Abrasive fine powder other than silica has high Mohs hardness due to alumina, chromium oxide, etc.
The end face of the optical fiber may be scratched, or there may be a step between the end face of the ferrule.If the Mohs altitude is low due to iron oxide, etc., the polishing power is insufficient and the surface is not smooth, resulting in a large return loss. Therefore, it is preferable to use an abrasive material equivalent to silica.

Further, there is a problem that the abrasive having a small average particle size has a low polishing force and requires a long time for polishing, and the abrasive having a large average particle size causes scratches (scratch scratches) on the polished surface. In addition, the surface is rough and the flatness is low, and there is a problem that it is not suitable for final polishing.

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 suitable for polishing an end face of a connector ferrule for an optical fiber by improving the dispersibility of a polishing material.

[0010]

A polishing body according to the present invention which has solved the above-mentioned problems is a polishing body in which a polishing layer containing fine abrasive powder and a binder is coated on a support. Average particle size of 0.01 to 4 as fine powder
It is characterized by using titanium oxide fine powder of μm, and the thickness of the support is 25 to 150 μm.

The polished body is particularly suitable for polishing the end face of a connector ferrule for an optical fiber.

The titanium oxide is desirably rutile.
Those having a Mohs hardness of 6 to 7, a specific gravity of 3.8 to 4.5, and an oil absorption of 5 to 50 ml / 100 g are preferred. The titanium oxide fine particles preferably have an average particle size of 0.01 to 4 μm, more preferably 0.1 to 4 μm.

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.

It is possible to polish the surface of the polishing layer while supplying a polishing liquid composed of water or a slurry (for example, 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.

[0016]

According to the polishing body of the present invention as described above, the abrasive of the polishing layer provided on the support having a thickness of 25 to 150 μm has a fine powder of titanium oxide having an average particle size of 0.01 to 4 μm. By using this, this titanium oxide fine powder is excellent in the dispersibility of the coating solution, it is uniformly dispersed in the binder without causing excessive aggregation and gelation of the particles, and the production efficiency is improved and the polishing is performed. The polishing layer obtained while the body is obtained at a low cost has a strong film quality, has the same Mohs hardness as silica particles, for example, when polishing the end face of the connector ferrule for optical fiber, the polishing performance is improved and the end face of the optical fiber is improved. Grinding flaws can be reduced.

That is, in the optical fiber connector ferrule whose end surface has been 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 so that no level difference occurs between them, and the return loss in light transmission when joining the polished end faces is reduced by -45.
It can be reduced to dB or less, and further, since there is no step, the end face is hardly stained.

In particular, when a titanium oxide fine powder having a rutile structure is used, the dispersibility and the surface properties of the polishing layer are improved.
It is suitable for finish polishing of an optical fiber connector ferrule. In addition, the coating liquid is dispersed by a sand grinder to obtain high dispersibility of fine silica powder,
In addition, a material obtained by adjusting the smoothness of the polishing layer surface by calendering treatment can obtain a suitable finish polishing characteristic.

In the polishing using the polishing body of the present invention, a polishing liquid using water or a slurry can be used if necessary, and a polishing liquid which provides lubricity and cooling properties and does not contain a base and an acid can be used. This facilitates waste liquid treatment.

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.

[0021]

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 0.01 to 4 μm (or 0.1 to 4 μm) and an oil absorption of 5 to 50 ml / min on a support 2 made of a polyester film or the like and having a thickness of 25 to 150 μm. A polishing layer 3 containing 100 g of a titanium oxide fine powder (abrasive) having a Rutile-type structure and a Mohs hardness of 6 to 7 and a binder (30 to 100 parts by weight with respect to 100 parts by weight of the silica fine powder) has a thickness of 5 to 25 μm. It is formed by laminating to a thickness, and 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 caused 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 or the like) 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 is for obtaining lubricity and cooling property of a polishing portion, does not contain a base or an acid, and in the case of a slurry, the average particle size of the abrasive contained in the slurry is such that the titanium oxide of the polishing layer 3 Those smaller than the average particle size of the fine powder are preferred.

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) is used to disperse and adjust the above-mentioned coating liquid for a polishing layer containing fine titanium oxide powder, a binder, a solvent and the like. Then, the 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 provided with a metal roll or a resin roll. The surface of the polishing layer is subjected to a calendering treatment by an apparatus, and if necessary, by a heat treatment apparatus. Then, it is formed into a predetermined shape by a punching process, a cutting process, or the like to form a polishing body.

As the fine abrasive powder used in the polishing layer of the present invention, the above-mentioned fine titanium oxide powder is used alone or together with another abrasive. Mohs hardness of 6 to 10 as other abrasives
And 30% or less of the total amount of powder. This abrasive is generally a material that has a polishing or polishing action,
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, silica, zirconia, cerium oxide, red iron oxide, garnet, etc., and materials having a Mohs hardness of 7 or more can be used in combinations of 1 to 4 types. These abrasives have an average particle size of 0.1 to 25μ.
A size of m is used. Specific examples of the abrasive include AKP1, AKP15, and AKP2 manufactured by Sumitomo Chemical Co., Ltd.
0, AKP30, AKP50, AKP80, Hit5
0, Hit100 and the like. These are described in JP-B-52-28642 and JP-B-49-39402.
No. JP-A-63-98828, U.S. Pat.
5, U.S. Pat. No. 3,077,807, U.S. Pat.
No. 96, U.S. Pat. No. 3,293,066, U.S. Pat.
No. 910, U.S. Pat. No. 3,833,412, U.S. Pat.
No. 7190, British Patent 1145349, West German Patent 85
No. 3211, etc.

Examples of the binder used in the polishing layer of the present invention include 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 carboxylic acid (COOM), sulfinic acid, sulfenic acid, sulfonic acid (SO ₃ M), phosphoric acid (PO) as functional groups other than the main functional groups. (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 (all 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.

Silicone oils (dialkyl polysiloxanes, dialkoxy polysiloxanes, phenyl polysiloxanes, fluoroalkyl polysiloxanes (KF96, KF69 manufactured by Shin-Etsu Chemical Co., Ltd.) can be used as organic compound-based lubricants.
)), 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 ethyl hexyl 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. No. 3,523,086, U.S. Pat. No. 3,625,760, U.S. Pat. No. 3,630,772, U.S. Pat. No. 3,634,253, 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.

The dispersant 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 a carbon number 1 to 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
metal soap (copper oleate), fatty acid amide, lecithin (soybean oil lecithin) or the like composed of 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 ester, phosphoric monoester, phosphoric diester, phosphoric triester, alkylphosphonic acid, phenylphosphonic acid, amine compound and the like can also be used. Further, polyethylene glycol, polyethylene oxide, sulfosuccinic acid, metal sulfosuccinate, 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.
Nos. 93 and 3470021.

As the antifungal agent used in the present invention, 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 compositions and the like, and applying 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, the coating liquid for the polishing layer can be prepared by kneading and dispersing according to the method described in the above-mentioned book or the literature cited therein.

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, impregnating 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, 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 at 20 ° C. (room temperature) to 130 ° C. in multiple stages, and the formed polishing layer is dried to a thickness of about 5 to 25 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. Examples of such wiping materials include various types of virgin manufactured by Japan Vilene Co., Ltd., Toraysee, Exaine manufactured by Toray Co., Ltd., Kimwipe (trade name), and various 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.

[0056]

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 4> Based on 100 parts of titanium oxide fine powder in the following polishing layer coating solution composition: A,
Mix binder and solvent except isocyanate,
This dispersion is placed in a sand grinder having a size of 0.25 gallon, 700 g of 1.2 mmφ glass beads are added, and the mixture is operated at 1,700 rpm for 150 minutes to be uniformly dispersed. Thereafter, the number of revolutions is reduced to 500 rpm, the viscosity is adjusted, and a coating liquid for a polishing layer mixed with a polyisocyanate (curing agent) is prepared. This coating solution was applied on a support made of a 75 μm-thick polyester film (PET) using a blade coater, and then dried to obtain a polished body having a dry coating film having a 15 μm-thick polishing layer formed thereon. This abrasive body was punched into a disk shape to obtain a sample as an abrasive sheet.

Examples 1 to 4 differ in the size of the abrasive.
Example 1 is a titanium oxide fine powder having an average particle size of 0.1 μm, Example 2 is a titanium oxide fine powder having an average particle size of 0.2 μm, and Example 3 is a titanium oxide fine powder having an average particle size of 0.3 μm. In Example 4, the average particle size was 1 μm.
Using fine powder of titanium oxide.

The polishing bodies of Examples 1 to 4 were adhered to 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 30 rpm, the revolution is 2 rpm,
Twelve connector ferrules were attached to the 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 60 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. The smoothness of the surface can be evaluated.
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 1-3> Table 1 shows Comparative Examples 1-3.
The results of the same polishing test performed on the polishing body of Example 1 are also shown. Comparative Example 1 is an example in which the material of the abrasive is chromium oxide and the average particle size is 0.5 μm. Comparative Example 2 is an example in which the material of the abrasive is iron oxide and the average particle size is 0.1 μm. 3 is made of alumina (# 8000)
And Comparative Examples 1 to 3 have the same coating liquid composition as Examples 1 to 4 except for the abrasive.

From the results shown in Table 1, in Examples 1 to 4 of the present invention, good results were obtained with respect to both the fiber surface damage and the return loss. On the other hand, in the case of the chromium oxide having a high Mohs hardness of Comparative Example 1, the fiber surface after polishing was damaged, and the return loss was large. In the case of the iron oxide having a low Mohs hardness of Comparative Example 2, the fiber surface was not damaged, but the return loss was large due to insufficient polishing. In the case of Comparative Example 3 using alumina fine powder having a high Mohs hardness, the fiber surface after polishing was damaged, and the return loss was large.

[Coating solution composition for polishing layer: A] Abrasive (material: X, average particle size: Y) 100 parts Binder (vinyl chloride resin, MR110: manufactured by Zeon Corporation) 20 parts Binder (sulfonate group-containing polyurethane) Resin, UR8200: Toyobo Co., Ltd. 30 parts Binder (polyisocyanate, Coronate L: Nippon Polyurethane Co., Ltd.) 40 parts MEK (methyl ethyl ketone) / Anon 150 parts Butyl acetate 50 parts

[0065]

[Table 1]

<Examples 5 to 8> The following coating liquid composition for a polishing layer: B was uniformly dispersed using a sand grinder in the same manner as in Examples 1 to 4, the viscosity was adjusted, and polyisocyanate (curing agent) was used. Is prepared, a coating liquid for a polishing layer is prepared, and the coating liquid is coated on a support made of a polyester film (PET) having a thickness of 30 to 125 μm, and then dried, and the dried coating film having a thickness of 10 μm is polished. An abrasive body having a layer formed thereon was obtained. This abrasive body was punched into a disk shape to obtain a sample as an abrasive sheet.

Examples 5 to 8 differ in the thickness of the support. Example 5 has a thickness of 30 μm, Example 6 has a thickness of 50 μm, and Example 7 has a thickness of 7 μm.
The thickness is 5 μm, and that of Example 8 is 125 μm.

The polishing bodies of Examples 5 to 8 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 12 rpm and the revolution is 2 rpm.
Twelve connector ferrules were attached to the 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 45 seconds. 1 cc of water (or slurry) was dropped on the polishing layer as a polishing liquid.

Table 2 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, together with the bonding characteristics of the polished body. Show.

The bonding property of the above-mentioned abrasive body is determined as follows. The thing that can be flatly attached by firmly fixing the back surface of the abrasive body on the elastic body of the base with water or a water-based adhesive using a surfactant is suitable. Acceptable: 、, unsuitable for those that cannot be applied flat without the use of an adhesive tape: determined to be ×.

<Comparative Examples 4 and 5> Table 2 also shows the results of similar polishing tests performed on the polished bodies of Comparative Examples 4 and 5. Comparative Example 4 is an example in which the thickness of the support is as thin as 20 μm, Comparative Example 5 is an example in which the thickness of the support is as thick as 200 μm, and in Comparative Examples 4 and 5, except for the thickness of the support, Example 5 was used. The composition of the coating liquid is the same as that of No. 8

From the results shown in Table 2, when the thickness of the support according to Examples 5 to 8 of the present invention is 30 to 125 μm, good results are obtained with respect to both the scratches on the fiber surface and the return loss, and the bonding characteristics are also improved. Appropriate and good adhesion was achieved. On the other hand, when the thickness of the support in Comparative Example 4 was as thin as 20 μm, the suitability for bonding was acceptable, but the abrasion body was wrinkled, the suitability for polishing was reduced, and the fiber surface after polishing was damaged, and the return loss was reduced. It is getting bigger. When the thickness of the support of Comparative Example 5 was as thick as 200 μm, there was no damage on the fiber surface, and the return loss was a good value comparable to that of Example 5. Met.

[Coating Composition for Polishing Layer: B] Abrasive (titanium oxide, average particle size: 0.3 μm) 100 parts Binder (polyester resin, CA118: manufactured by Morton) 40 parts Binder (polyurethane resin containing sulfonic acid group, UR8200: Toyobo Co., Ltd. 30 parts Binder (polyisocyanate, Coronate L: Nippon Polyurethane Co., Ltd.) 20 parts MEK (methyl ethyl ketone) / Anon 150 parts Xylene 50 parts

[0074]

[Table 2]

[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

Claims (5)

[Claims] 1. A polishing body in which a polishing layer containing a fine abrasive powder and a binder is coated on a support, wherein the fine abrasive powder of the polishing layer has an average particle size of 0.
A polished body, characterized by using fine titanium oxide powder of 01 to 4 μm and having a thickness of the support of 25 to 150 μm. 2. The polishing body according to claim 1, wherein the polishing body is for polishing an end surface of an optical fiber connector ferrule. 3. The polishing body according to claim 1, wherein the titanium oxide is of a rutile type. 4. The polishing body according to claim 1, wherein the application liquid for applying the polishing layer is dispersed by using a sand grinder. 5. The polishing body according to claim 1, wherein a calendering treatment is performed on a surface of the polishing layer.