JPH09155748A - Polishing body for ultra-low reflected light connector ferrule - Google Patents

Abstract

PROBLEM TO BE SOLVED: To improve surface smoothness and transmitting efficiency with low reflection for a polishing body used to polish the end of an optical connector ferrule by providing a flexible support with a polishing layer formed of abrasives and a cellulose resin binder and with a specified center-line average surface roughness. SOLUTION: A polishing body used to polish an optical connector ferrule has a polishing layer formed of abrasives and a cellulose resin contained binder on the single face of a flexible support, with a center-line average surface roughness being 0.01-0.05μm. In this way, while the optical connector ferrule has the end formed to be a convex spherical face as desired and a ferrule surface and an optical fiber surface are smoothed, polishing is possible without level differences and ultra-low reflecting property and more transmitting efficiency are provided for an optical connector. During polishing, a coolant is supplied to the surface of the polishing layer. The coolant contains polishing particles such as silica.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polishing sheet, a polishing disk, etc. used for finishing polishing the tip of an optical connector ferrule having an optical fiber inserted and fixed in a ferrule hole into a convex spherical surface having an ultra-low reflection characteristic. It relates to an abrasive body.

[0002]

2. Description of the Related Art As a technique for polishing the tip of an optical connector ferrule in which an optical fiber is inserted and fixed in a ferrule hole as described above to a convex spherical surface, conventionally, various methods using a polishing sheet or a free abrasive grain holding film have been used. Is proposed.

As an example, as disclosed in Japanese Unexamined Patent Publication No. 3-81708, a certain tension is applied to a cellulosic resin film containing no abrasive, and the tip of an optical connector ferrule is pressed against the surface of this resin film. A polishing method has been proposed in which, while sliding, a coolant liquid containing a silica-based polishing agent is supplied to the contact portion to perform polishing.

[0004]

However, in the above-mentioned polishing of the optical connector ferrule, the smoothness is maintained between the ferrule surface and the optical fiber surface, and the step is not generated between the ferrule surface and the optical fiber surface. It was very difficult to obtain ultra-low reflection characteristics.

In particular, the difference in polishing characteristics between the ferrule made of a ceramic material and the optical fiber made of a glass material is caused by the difference in material, and in order to polish the tip into a convex spherical surface, the polishing body is held in an elastic state for polishing, etc. Due to the reason, it is difficult to grind into a desired shape, and management of grinding conditions becomes complicated.

The present invention has been made in view of the above points, and an object thereof is to provide a polishing body suitable for polishing the tip of an optical connector ferrule.

[0007]

The polishing body of the present invention, which has solved the above-mentioned problems, comprises a flexible support provided with a polishing layer comprising an abrasive and a binder, and the center line average surface roughness of the polishing layer. Ra (JIS-B-R0601-1982) is 0.
It is characterized in that it is from 01 to 0.05 μm, preferably 0.025 μm or less, and a cellulose resin is used as a binder.

The center line average surface roughness Ra of the polishing layer is
If it is smaller than 0.01 μm and smoother, the polishing power is low and the polishing time becomes too long, and if it is larger than 0.05 μm and it is rough, the smoothness of the optical connector ferrule surface after polishing is insufficient and the light amount transferability becomes poor. If it is lowered or a large step is generated between the optical fiber surface and the ferrule surface, desired ultra-low reflection characteristics cannot be obtained.

Nitrocellulose is preferred as the cellulosic resin used as the binder in the polishing layer. The 100% modulus is preferably more than 500 Kg / cm ² . The number average molecular weight is 10,000 to 10
0000 is preferred. The above cellulose-based resin is preferably used in an amount of 30% by weight or more based on the total binder.

As the polishing agent, alumina oxide, chromium oxide and iron oxide are particularly preferable, and the particle diameter thereof is 0.1 to 1 μm.
m is preferred. The compounding amount of the abrasive and the binder is in the range of 5 to 150 parts by weight, preferably 10 to 110 parts by weight, with respect to 100 parts by weight of the abrasive. Further, the polishing layer may contain carbon black.

The flexible support is preferably polyester such as polyethylene terephthalate or polyethylene naphthalate, and preferably has a thickness of 50 to 300 μm.

The polishing body as described above has a center line average surface roughness Ra of the polishing layer surface of 0.01 to 0.05 μm,
Since the polishing body is extremely smooth, in order to obtain such a surface roughness Ra, the polishing layer is laminated on the flexible support and then the surface is smoothed by calendering, or the polishing layer is formed. The time for dispersing the coating liquid for the polishing layer constituting the above is made 2 to 10 times longer than that for the normal one, thereby smoothing the surface of the polishing layer. The calendar molding is, for example,
A polishing body is inserted between the elastic roll and the heated metal roll, and the surface is smoothed by heat and pressure.

To polish the tip of an optical connector ferrule using the polishing body according to the present invention, a polishing body (polishing sheet or the like) is attached to a rotary table made of an elastic body such as rubber, and the tip of the optical connector ferrule is attached to this polishing body. Press contact
While rotating the rotary table, the optical connector ferrule is planetarily moved and polished.

At this time, a dry method may be used, but a wet method is preferable. For the wet type, it is preferable to supply an aqueous coolant solution, and polishing fine particles (silica, alumina, etc.) are contained in this coolant solution.
May be included. In the case of silica, colloidal silica is suitable and its particle size is 0.005-0.05 μm.
A degree is desirable. The polishing time is preferably 5 to 200 seconds and the load is preferably 1 to 1000 g.

[0015]

According to the present invention as described above, the center line average surface roughness Ra of the polishing layer provided on the flexible support is 0.0.
1 to 0.05 μm, and by using a cellulosic resin as the binder, the tip of the optical connector ferrule can be formed into a desired convex spherical surface without causing a step while ensuring smoothness of the ferrule surface and the optical fiber surface. It can be polished, and it has an ultra-low reflection property as an optical connector, improves the transmission efficiency, and can be easily polished.

In particular, when the binder contains a cellulosic resin, it has good dispersibility and contributes to smoothing of the surface, and when it has hydrophilicity and contains free abrasive grains in the coolant, The retention of abrasive grains between the surface of the polishing layer and the tip of the optical connector ferrule is good, and good polishing characteristics can be obtained in combination with the hardness of the polishing layer.

[0017]

BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in more detail below with reference to an embodiment of a polishing body for an ultra-low reflection optical connector ferrule of the present invention.

The polishing body (polishing sheet) of this example has a polishing layer composed of a polishing agent and a binder containing at least a cellulosic resin on one surface of a flexible support. Ra is formed to 0.01 to 0.05 μm. An undercoat layer may be provided between the flexible support and the polishing layer, and a back layer may be provided on the back surface of the support.

The polishing agent used in the polishing layer is generally a material having a polishing action or a polishing action, and is made of α-alumina, γ-alumina, α · γ-alumina, fused alumina,
Silicon carbide, chromium oxide, cerium oxide, corundum, artificial diamond, diamond, α-iron oxide, garnet, emery (main component: corundum and magnetite), garnet, silica, silicon nitride, boron nitride, molybdenum carbide, boron carbide, Tungsten carbide, titanium carbide, tripoly, diatomaceous earth, dolomite, and the like, and materials having a Mohs hardness of 6 or more are mainly used in combinations of 1 to 4 types.

These abrasives have an average particle size of 0.1.
Those having a size of ˜1.0 μm are used, and particularly preferably 0.1 to 0.6 μm. In the case of an abrasive layer, these abrasives contain 5 parts by weight of a binder per 100 parts by weight of the abrasive.
It is used in an amount of up to 150 parts by weight, preferably 10 to 110 parts by weight.

Specific examples of these abrasives include AKP1, AKP15, AKP20, AKP30, manufactured by Sumitomo Chemical Co., Ltd.
AKP50, AKP80, Hit50, Hit100, etc. are mentioned. About these, Japanese Patent Publication No. 52-2864
2, JP-B-49-39402, JP-A-63-988.
28, U.S. Pat. No. 3687725, U.S. Pat. No. 3007
807, U.S. Pat. No. 3,041,196, U.S. Pat.
3066, U.S. Pat. No. 3,630,910, U.S. Pat. No. 38
No. 33412, U.S. Pat. No. 4,117,190, British Patent 1
145349, West German Patent 853211 and the like.

As the binder used in the polishing layer of the present invention, a cellulosic resin is used. In addition to the cellulosic resin, conventionally known thermoplastic resin, thermosetting resin, reactive resin, electronic A line curable resin, an ultraviolet curable resin, a visible light curable resin or a mixture thereof is used.

As the cellulose resin (cellulose derivative), cellulose acetate butyrate, cellulose diacetate, cellulose triacetate, cellulose propionate, nitrocellulose, ethyl cellulose, methyl cellulose, propyl cellulose, methyl ethyl cellulose, carboxymethyl cellulose, acetyl cellulose, etc. Can be mentioned.

Other thermoplastic resins include those having a softening temperature of 150 ° C. or lower and an average molecular weight of 10,000 to 30,000.
0, the degree of polymerization is about 50 to 2000, more preferably about 200 to 600, for example, vinyl chloride vinyl acetate copolymer, vinyl chloride copolymer, vinyl chloride vinyl acetate vinyl alcohol copolymer, vinyl chloride. Vinyl alcohol copolymer, vinyl chloride chloride vinylidene chloride copolymer, vinyl chloride acrylonitrile copolymer, acrylic ester acrylonitrile copolymer, acrylic ester vinylidene chloride copolymer, acrylic ester styrene copolymer, methacrylic ester acrylonitrile Copolymers, Methacrylic Acid Ester Vinylidene Chloride Copolymers, Methacrylic Ester Styrene Copolymers, Urethane Elastomers, Nylon-Silicon Resins, Nitrocellulose-Polyamide Resins, Poly (Fucca Vinyl), Vinylidene Acrylonitrile Copolymers, butadiene acrylonitrile copolymers, polyamide resins, polyvinyl butyral, styrene butadiene copolymers, polyester resins, polycarbonate resins, chlorovinyl ether acrylate copolymers, amino resins, various synthetic rubber thermoplastic resins, and A mixture of these is used.
Examples of these resins include JP-B-37-6877, JP-B-39-12528, JP-B-39-19292, JP-B-40-5349, JP-B-40-20907, JP-B-41-9463 and JP-B-41-9463. JP-B-41-14059, JP-B-41-16985, JP-B-42-6428, JP-B-42-11621, JP-B-43-4623, JP-B-43-15206, JP-B-44-2889, JP-B-44-8989 44-17947, Japanese Patent Publication No. 44-18232,
Japanese Patent Publication No. 45-14020, Japanese Patent Publication No. 45-14500
Issue, Japanese Examined Patent Publication No. 47-18573, Japanese Examined Patent Publication No. 47-2206
No. 3, Japanese Patent Publication No. 47-22064, Japanese Patent Publication No. 47-220
No. 68, Japanese Patent Publication No. 47-22069, Japanese Patent Publication No. 47-22
070, Japanese Patent Publication No. 47-27886, and Japanese Patent Laid-Open No. 57-1.
33521, JP-A-58-137133, JP-A-5
8-166533, JP-A-58-222433, JP-A-59-58642, and the like, US Pat. No. 4,571,364.
And US Pat. No. 4,752,530.

The thermosetting resin or reactive resin has a molecular weight of 200,000 or less in the state of a coating liquid, and the molecular weight becomes infinite due to a reaction such as condensation / addition by heating and humidifying after coating and drying. Is suitable. Further, among these resins, those that do not soften or melt before the resin is thermally decomposed are preferable. Specifically, for example, phenol resin, phenoxy resin, epoxy resin,
Polyurethane resin, polyester resin, polyurethane polycarbonate resin, urea resin, melamine resin, alkyd resin, silicone resin, acrylic reaction resin (electron beam curing resin), epoxy-polyamide resin, nitrocellulose melamine resin, high molecular weight polyester resin and isocyanate prepolymer Polymer mixture, methacrylate copolymer and diisocyanate prepolymer mixture, polyester polyol and polyisocyanate mixture, urea formaldehyde resin, low molecular weight glycol / high molecular weight diol / triphenylmethane triisocyanate mixture, polyamine resin, polyimine Resins and mixtures thereof. Examples of these resins include Japanese Patent Publication No. 39-8.
No. 103, Japanese Patent Publication No. 40-9779, Japanese Patent Publication No. 41-71
No. 92, Japanese Patent Publication No. 41-8016, Japanese Patent Publication No. 41-142
No. 75, Japanese Patent Publication No. 42-18179, Japanese Patent Publication No. 43-12
081, No. 44-28023, No. 45-1
4501, Japanese Patent Publication No. 45-24902, Japanese Patent Publication No. 46-
13103, Japanese Patent Publication No. 47-22065, Japanese Patent Publication No. 47
-22066, Japanese Patent Publication No. 47-22067, Japanese Patent Publication No. 4
No. 7-22072, JP-B-47-22073, JP-B-47-28045, JP-B-47-28048, JP-B-47-28922 and the like.

In addition to the main functional groups, these thermoplastic resins, thermosetting resins and reactive resins have carboxylic acid (COOM), sulfinic acid, sulfenic acid, sulfonic acid (SO ₃ M) and phosphoric acid (COOM) as functional groups. PO (OM) (OM)),
Phosphonic acid, sulfuric acid (OSO ₃ M), acidic groups such as ester groups (M is H, alkali metal, alkaline earth metal, hydrocarbon group), amino acids; aminosulfonic acids,
Sulfuric acid or phosphoric acid esters of amino alcohols, amphoteric groups such as alkyl betaine type, amino groups, imino groups, imide groups, amide groups, etc., and also hydroxyl groups, alkoxyl groups, thiol groups, alkylthio groups, halogen groups (F, Cl , B
r, 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 are usually contained in 1 to 6 types, and each functional group is 1 per 1 g of resin. × 10 ^-6 eq ~ 1 × 10
^-2 eq is preferred.

These binders may be used alone or in combination, and other additives may be added. Additives include dispersants, lubricants, abrasives, antistatic agents, antioxidants, solvents and the like. In addition, the mixing ratio of the powder agent and the binder in the back layer is in the range of 8 to 400 parts by weight of the binder with respect to 100 parts by weight of the fine powder.

The polyisocyanates used in the polishing layer of the present invention include tolylene diisocyanate, 4.4'-diphenylmethane diisocyanate, hexamethylene diisocyanate, xylylene diisocyanate, naphthylene-1.5-diisocyanate, o-toluidine diisocyanate, isophorone diisocyanate. Isocyanates such as triphenylmethane triisocyanate and isophorone diisocyanate, products of the isocyanates and polyalcohols, polyisocyanates of 2 to 10 mer produced by condensation of isocyanates, products of polyisocyanates and polyurethanes. It is possible to use those whose terminal functional group is isocyanate.

The average molecular weight of these polyisocyanates is preferably 100 to 20,000. Commercially available product names of these polyisocyanates are Coronate L, Coronate HL, Coronate 2030, Coronate 2031, Millionate MR, Millionate MT.
L (manufactured by Nippon Polyurethane Company), Takenate D-102,
Takenate D-110N, Takenate D-200, Takenate D-202, Takenate 300S, Takenate 5
00 (manufactured by Takeda Pharmaceutical Co., Ltd.), Sumidule T-80, Sumidule 44S, Sumidule PF, Sumidule L, Sumidule N, Death Module L, Death Module I
L, Death module N, Death module HL, Death module T65, Death module 15, Death module R, Death module RF, Death module SL, Death module Z4273 (manufactured by Sumitomo Bayer), etc. It can be used in combination of two or more utilizing the difference of. Further, for the purpose of accelerating the curing reaction, hydroxyl groups (butanediol, hexanediol, molecular weight of 1000-10
000 polyurethane, water, etc.), a compound having an amino group (monomethylamine, dimethylamine, trimethylamine, etc.), a metal oxide catalyst, or a catalyst such as iron acetylacetonate can be used together. It is desirable that these compounds having a hydroxyl group or an amino group are polyfunctional.
These polyisocyanates are preferably used in both the polishing layer and the back layer in an amount of 2 to 70 parts by weight, more preferably 5 to 50 parts by weight, based on 100 parts by weight of the total amount of the binder resin and the polyisocyanate. Examples of these are shown in JP-A-60-131622 and JP-A-61-74138.

Carbon black may be contained in the polishing layer. For example, a furnace for rubber, a thermal for rubber, a black for color, an acetylene black and the like can be used. Its specific surface area is 5-500 m ² / g, D
BP oil absorption is 10-400 ml / 100g, pH is 2-
10, water content 0.1 ~ 10%, tap density 0.1 ~
It is preferably 1 g / cm ² . As a specific example of this carbon black, manufactured by Cabot: BLACK
PEARLS 2000, 1300, 1000, 90
0,800,700, Mitsubishi Kasei Co., Ltd .: 650B, 9
50B, 3250B, 850, 900, 960, 98
0,1000,2300,2400,2600 etc. are mentioned. 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 powdery lubricant used in the polishing layer of the present invention, graphite, molybdenum disulfide, boron nitride, graphite fluoride, calcium carbonate, barium sulfate, silicon oxide, titanium oxide, zinc oxide, tin oxide, Inorganic fine powder such as tungsten disulfide, acrylic styrene resin fine powder, benzoguanamine resin fine powder, melamine resin fine powder,
Resin fine powder such as polyolefin fine resin fine powder, polyester fine resin fine powder, polyamide fine resin fine powder, polyimide fine resin fine powder, and polyfuccaethylene fine resin fine powder.

As organic compound-based lubricants, silicone oils (dialkyl polysiloxane, dialkoxy polysiloxane, phenyl polysiloxane, fluoroalkyl polysiloxane (KF96, KF69 manufactured by Shin-Etsu Chemical Co., Ltd.)
Etc.)), fatty acid modified silicone oil, fluorine alcohol, polyolefin (polyethylene wax, polypropylene etc.), polyglycol (ethylene glycol, polyethylene oxide wax etc.), tetrafluoroethylene oxide wax, polytetrafluoroglycol, perfluoroalkyl ether, perfluoro Compounds with fluorine or silicon introduced such as fatty acid, perfluoro fatty acid ester, perfluoroalkyl sulfate ester, perfluoroalkyl sulfonate ester, perfluoroalkylbenzene sulfonate ester, perfluoroalkyl phosphate ester, alkyl sulfate ester, alkyl sulfonate ester , Alkylphosphonic acid triester,
Organic acids and organic acid ester compounds such as alkylphosphonic acid monoester, alkylphosphonic acid diester, alkylphosphoric acid ester, succinic acid ester, triazaindolizine, tetraazaindene, benzotriazole, benzotriazine, benzodiazole, EDTA, etc. Heterocyclic compounds containing nitrogen and sulfur, C10-4
0 monobasic fatty acids and any one or more of monohydric alcohols having 2 to 40 carbon atoms or dihydric alcohols, trihydric alcohols, tetrahydric alcohols, and hexahydric alcohols Fatty acid esters, C10
Or more monobasic fatty acids and fatty acid esters consisting of monovalent to hexavalent alcohols having 11 to 70 carbon atoms in total with the carbon number of the fatty acids, fatty acids having 8 to 40 carbon atoms or fatty acid amides , Fatty acid alkylamides, and fatty alcohols can also be used.

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, Alkylamido 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.

As the lubricant used in the present invention,
So-called lubricating oil additives can be used alone or in combination, and antioxidants known as rust preventives (alkylphenol, benzotriazine, tetraazaindene,
Sulfamide, guanidine, nucleic acid, pyridine, amine,
Hydroquinone, metal chelating agents such as EDTA), rust-suppressing agents (naphthenic acid, alkenylsuccinic acid, phosphoric acid, dilauryl phosphate, etc.), oiliness agents (rapeseed oil, lauryl alcohol, etc.), extreme pressure agents (dibenzyl sulfide, Tricresyl phosphate, tributyl phosphite, etc.),
Detergent dispersants, viscosity index improvers, pour point depressants, foam depressants, etc. These lubricants are added in the range of 0.01 to 30 parts by weight based on 100 parts by weight of the binder. About these, Japanese Patent Publication No. 43-23889 and Japanese Patent Publication No. 48
-24041, Japanese Patent Publication No. 48-18482, Japanese Patent Publication No. 4
4-18221, JP-B-47-28043, JP-B-57-56132, JP-A-59-8136, JP-A-59-8139, JP-A-61-85621, US Pat. No. 3,423,233, US Patent 3470021, U.S. Pat. No. 3,492,235, U.S. Pat. No. 3,497,411, U.S. Pat. No. 3,523,086, U.S. Pat. No. 3,625,760,
US Pat. No. 3,630,772, US Pat. No. 3,634,253
U.S. Pat. No. 3642539, U.S. Pat. No. 368772
5, US Patent No. 4135031, US Patent No. 44978
64, US Pat. No. 4,552,794, IBM Technical Disclosure Bulletin (IBM Tech).
natural Disclosure Bulleti
n) Vol. 9, No7, p779 (12, 1966)
Mon), ELEKTRONIK 196
1st year No12, p380, "Chemical Handbook (Application)" p9
54-967, published by Maruzen in 1980.

Examples of the dispersant and dispersion aid 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 and stearolic acid. , Behenic acid, maleic acid, phthalic acid, etc., fatty acid having 2 to 40 carbon atoms (R ₁ COOH, R ₁ is alkyl group having ₁ to 39 carbon atoms, phenyl group, aralkyl group), alkali metal of the above fatty acid (Li, Na, K, NH ₄ ^+, etc.) or alkaline earth metal (Mg, Ca, Ba, etc.), metal soap made of Cu, Pb, etc. (copper oleate), fatty acid amide; lecithin (soybean oil lecithin), etc. Is used. Besides, higher alcohols having 4 to 40 carbon atoms (butanol, octyl alcohol, myristyl alcohol, stearyl alcohol) and their sulfuric acid esters, sulfonic acids, phenylsulfonic acids, alkylsulfonic acids, sulfonic acid esters, phosphoric acid monoesters, phosphoric acid diesters , Phosphoric acid triester, alkylphosphonic acid, phenylphosphonic acid, amine compounds and the like can also be used. Further, polyethylene glycol, polyethylene oxide, sulfosuccinic acid, sulfosuccinic acid metal salt, sulfosuccinic acid ester and the like can also be used. One or more of these dispersants are usually used, and one type of dispersant is used in an amount of 0.0 to 100 parts by weight of the binder.
It is added in the range of 0.5 to 20 parts by weight. The method of using these dispersants may be such that they are pre-deposited on the surface of the abrasive or non-abrasive fine powder, or they may be added during the dispersion. Such a material is disclosed, for example, in Japanese Examined Patent Publication No. 39-28369 and Japanese Examined Patent Publication No. 4
No. 4-17945, Japanese Patent Publication No. 44-18221, Japanese Patent Publication No. 48-7441, Japanese Patent Publication No. 48-15001, Japanese Patent Publication No. 48-15002, Japanese Patent Publication No. 48-16363, Japanese Patent Publication No. 49-39402, and U.S. Pat. No. 3,387,993. No. 3470021 and the like.

The antifungal agent used in the present invention includes 2- (4
-Thiazolyl) -benzimidazole, N- (fluorodichloromethylthio) -phthalimide, 10 · 10'-
Oxybisphenoxarcin, 2, 4, 5, 6 tetrachloroisophthalonitrile, P-tolyldiiodomethylsulfone, triiodoallyl alcohol, dihydroacetate, 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).

Antistatic agents other than carbon black used in the present invention include graphite, modified graphite,
Conductive powder such as carbon black graft polymer, tin oxide-antimony oxide, tin oxide, titanium oxide-tin oxide-antimony oxide; natural surfactant such as saponin; alkylene oxide type, glycerin type, glycidol type, 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, phosphonium or sulfonium compounds, etc. Cationic surfactants; anionic surfactants containing acidic groups such as carboxylic acid, sulfonic acid, phosphonic acid, phosphoric acid, sulfuric acid ester group, phosphonic acid ester, phosphoric acid ester group; amino acids; amino sulfonic acids, sulfuric acid of amino alcohol Other 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.
No. 88226, No. 2676122, No. 2676924
Nos. 2,697,975, 2,691,566, 27
27860, 2730498 and 2742379.
No. 2, ibid. 2739891, ibid. 3068101, ibid. 31
58484, 3203203, 3210191
No. 3294540, No. 3415649, No. 34
41413, 3444254, 3475174
No. 3,545,974, West German Patent Publication (OLS) 19
No. 42665, British Patent No. 1077317, No. 1198.
No. 450, Ryohei Oda et al., “Synthesis of surfactants and their applications” (Maki Shoten 1972 edition); W. Bairi's "Surfs Active Agents" (Interscience Publications 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"
It is described in written books such as Koshobo (1968).

These surfactants may be added alone or as a mixture. The amount of these surfactants used in the polishing layer is 0.01-10 per 100 parts by weight of the polishing agent.
Parts by weight. The amount used in the back layer is binder 1
It is 0.01 to 30 parts by weight per 00 parts by weight. Although these are used as antistatic agents, they are sometimes used for other purposes such as improving dispersion, improving lubricity, coating aids, wetting agents, curing accelerators, and dispersion accelerators. .

As the organic solvent used in the dispersion, kneading and coating of the present invention, a ketone system such as acetone, methyl ethyl ketone, methyl isobutyl ketone, cyclohexanone, isophorone and tetrahydrofuran in any ratio; methanol, ethanol, propanol, butanol , Alcohol such as isobutyl alcohol, isopropyl alcohol, and methylcyclohexanol; methyl acetate,
Ester systems such as ethyl acetate, butyl acetate, isobutyl acetate, isopropyl acetate, ethyl lactate, glycol acetate monoethyl ether, etc .; ether systems such as diethyl ether, tetrahydrofuran, glycol dimethyl ether, glycol monoethyl ether, dioxane; benzene, toluene, xylene, Tar-based compounds (aromatic hydrocarbons) such as cresol, chlorobenzene and styrene; chlorinated hydrocarbons such as methylene chloride, ethylene chloride, carbon tetrachloride, chloroform, ethylene chlorohydrin and dichlorobenzene, N ・ N-dimethylformaldehyde , Hexane, etc. can be used. Further, these solvents are usually used in two or more kinds at an arbitrary ratio. In addition, trace amounts of impurities (polymerization of the solvent itself, water,
Raw material components).

These solvents have a total solid content of 1% of the polishing coating solution.
It is used in an amount of 50 to 20000 parts by weight with respect to 00 parts by weight. The solid content of the polishing coating liquid is preferably 5 to 60% by weight. Aqueous solvent (water, alcohol,
Acetone etc.) can also be used.

The polishing layer is formed by dissolving the above composition in any combination, dissolving it in an organic solvent, and coating and drying it as a coating solution on a support. This support is flexible and has a thickness of 50
About 300 μm. Materials include polyesters such as polyethylene terephthalate and polyethylene naphthalate, polyolefins such as polypropylene, cellulose derivatives such as cellulose triacetate and cellulose diacetate, vinyl resins such as polyvinyl chloride, polycarbonate, polyimide, polyamide, polysulfone, etc. In addition to the above plastics, metals such as aluminum and copper and ceramics such as glass can 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. Regarding these supports, for example, West German Patent 3338854A, JP-A-59-
116926, JP-A 61-129731, U.S. Pat. No. 4,388,368; Yukio Mitsuishi, "Fiber and Industry," Vol. 31, p50-55, 1975. The center line average surface roughness Ra of these supports is 0.001 to 5.
0 μm is preferred. The Young's modulus of these supports (F5
The value) is 2 to 30 kg in both width and length depending on the purpose.
/ Mm ² (1 Kg / 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. An ordinary kneading machine is used for preparing the polishing coating solution, for example, a two-roll mill, a three-roll mill, a ball mill, a pebble mill, a tron mill, a sand grinder, a Szegvari attritor, a high speed impeller, a dispersing machine, a high speed stone mill, a high speed mill. Impact mill, Disper, Kneader, High speed mixer, Ribbon blender, Cokneader, Intensive mixer,
A tumbler, a blender, a disperser, a homogenizer, a single screw extruder, a twin screw extruder, an ultrasonic disperser, etc. can be used. Usually, dispersion / kneading is equipped with a plurality of these dispersion / kneading machines,
Process continuously. For more information on kneading and dispersing technology,
T. C. PATTON (T.C.Patton) "P
aint Flow and Pigment Dis
"Person" (Paint Flow and Pigment Dispersion), 1964, John Wil
Published by ey & Sons (John Willie and Sons) and Shinichi Tanaka, "Industrial Materials," Vol. 25, 37 (1)
977), etc., and cited documents of the book.
As an auxiliary material for the dispersion and kneading, in order to efficiently carry out the dispersion and kneading, the equivalent spherical diameter is 10 cmφ to 0.05 mmφ
It is possible to use steel balls, steel beads, ceramic beads, glass beads, and organic polymer beads having the same diameter. These materials are not limited to spherical shapes. It is also described in specifications such as U.S. Patent Nos. 2,581,414 and 2,855,156. Also in the present invention, the polishing coating solution can be prepared by kneading and dispersing according to the method described in the above-mentioned book or the references cited in the book.

The surface roughness of the surface of the polishing layer coated and formed on the support can be adjusted by adjusting the dispersion / kneading processing time (dispersion time). In order to do so, the dispersion time is set long.

As a method for coating the above-mentioned coating liquid for the polishing layer on the support, the viscosity of the coating liquid is adjusted to 1 to 20000 centistokes (25 ° C.), and an air doctor coater, a blade coater, an air knife coater, and a squeeze coat are used. Coater, impregnation 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, and detailed explanations of these can be found in "Coating Engineering", pages 253-2, published by Asakura Shoten
It is described in detail on page 77 (published 46.20. Showa) and the like. The order of applying these coating liquids can be arbitrarily selected, and corona discharge treatment or the like may be performed before the application of the desired liquid to improve the adhesion to the undercoat layer or the support. The multilayer structure of the polishing layer may be a simultaneous multilayer coating, a sequential multilayer coating, or the like. These are described, for example, in
-123532, JP-B-62-37451, JP-A-59-142741, JP-A-59-1
No. 65239, and the like.

By such a method, about 1 to about 1 is formed on the support.
If necessary, the polishing liquid applied with a thickness of about 200 μm is immediately subjected to a multi-stage drying treatment at 20 to 130 ° C., and then the formed polishing layer is dried to a thickness of 0.05 to 10 μm. The transport speed of the support at this time is usually 10 m / min to 900.
The drying temperature is 20 ° C in multiple drying zones.
Controlling at ~ 130 ° C, the residual solvent amount of the coating film is 0.1-4.
It is set to 0 mg / m ² . If necessary, the surface of the polishing layer or the back layer is subjected to surface smoothing so that the center line average surface roughness is 0.001 to 0.05 μm (cutoff is 0.08 m).
m), preferably 0.001 to 0.025 μm, and cut into a desired shape to produce the abrasive body of the present invention. These manufacturing methods include powder pretreatment / surface treatment, kneading / dispersion, coating / drying, smoothing treatment, heat treatment, EB treatment,
It is desirable to continuously perform the steps of surface polishing, cutting and winding.

The smoothing treatment is also called calendering treatment and can smooth the polishing layer. As the calender, a metal roll, a nylon roll, a resin roll such as an epoxy roll can be used. Treatment temperature is 30 to 100 ° C, load is 50 to
It is preferably performed at 300 Kg / cm, and the smoothness changes depending on the temperature and load conditions. If it is performed in multiple stages, the processing is completed quickly. These are, for example, Japanese Patent Publication No. 40-23625.
No., JP-B-39-28368, JP-B-47-3880
No. 2, British Patent No. 1191424, Japanese Patent Publication No. 48-113
No. 36, JP-A-49-53631, JP-A-50-11
No. 2005, JP-A-51-77303, Japanese Patent Publication No. 52-
No. 17404, 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 thus-prepared abrasive body is cut or punched into a predetermined shape. It is desirable to perform burnishing and / or cleaning of the polishing body in the process before this. Burnish concretely polishes the polishing body with a hard material such as a sapphire blade, a razor blade, a super hard material blade, a diamond blade, and a ceramics blade, and smoothes the protrusions on the surface of the polishing body. 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 have to be a blade in particular, and a shape such as a square shape, a round shape, or a wheel (these materials may be provided around a rotating cylindrical shape) can also be used. Further, cleaning of the polishing body is performed by wiping the surface of the polishing body with a non-woven fabric or the like for the purpose of removing dirt on the surface of the polishing body and excess lubricant. Examples of such wiping materials include various types of Vilene made by Japan Vilene, Toraysee made by Toray, Exaine,
Product name Kimwipe, various polishing tapes made by Fuji Photo Film, non-woven fabric made of nylon, non-woven fabric of polyester, non-woven fabric of rayon, non-woven fabric of acrylonitrile,
Tissue paper such as non-woven fabric can be used.
These are, for example, Japanese Patent Publication Nos. 46-39309 and 58.
-46768, JP-A-56-90429, JP-B-5
No. 8-46767, JP-A-63-259830, JP-A-1-201824 and the like.

Abrasives, binders used in the present invention,
Additives (lubricants, dispersants, antistatic agents, surface treatment agents, carbon black, abrasives, light-shielding agents, antioxidants, antifungal agents, etc.), solvents and supports (undercoat layer, back layer, back bottom) A coating layer may be provided) or its production method can be referred to the production method of an abrasive body described in JP-B-56-26890.

[0050]

EXAMPLES Examples and comparative examples of the present invention will be shown below to evaluate the polishing characteristics. The term "parts" in the examples means "parts by weight".

<Examples 1 to 5> In the polishing body of this example, a polishing coating solution prepared by the following composition A was bar-coated on a polyester support having a thickness of 75 μm to a thickness of 3 μm to form a polishing layer. Formed. In Examples 1 to 5, the blending amount of the nitrocellulose resin in all the binders was changed.

The above-mentioned polishing body (polishing sheet) has a diameter of 200.
punched into a disc shape of mm and attached on a rubber rotary plate, and while rotating this rotary plate at 100 rpm, the optical connector ferrule is caused to make a planetary motion on it and the tip is brought into contact with the polishing layer to perform polishing for 20 seconds. It was As the supplied coolant liquid, an aqueous solution containing colloidal silica having a particle diameter of 0.02 μm was used.

The mixing ratio of the binder in the polishing body, the measurement result of the surface roughness Ra of the polishing layer, the measurement result of the step between the ferrule surface and the optical fiber surface, and the measurement result of the light quantity transmission loss of the polished optical connector ferrule were obtained. It shows in Table 1.

The light quantity transmission loss is obtained by measuring the loss quantity of the transmitted light quantity caused by the reflection on the polished surface of the optical fiber.
The smoothness of the surface can be evaluated, and the larger the dB value, the smaller the transmission loss and the better the transmission state. The step difference is obtained by polishing silica glass as an optical fiber and zirconia as a ferrule and measuring the step difference between the surfaces. The smaller the value, the better.

<Comparative Examples 1 and 2> Table 1 also shows the test results of Comparative Examples 1 and 2. In this comparative example, a coating solution having the same composition was applied to a support similar to that of the above-mentioned example, but a polishing layer containing no nitrocellulose resin (Comparative Example 1) was used. It is not contained (Comparative Example 2).

[Coating liquid composition: A] Abrasive (chromium oxide, average particle size 0.5 μm): 30 parts Binder (nitrocellulose resin): X part Binder (polyester polyurethane, sulfonic acid group 3 × 10 ⁻³ equivalent / g, epoxy group 2 × 10 ⁻⁵ equivalent / g): Y part Binder (polyisocyanate, TDI (3 mol) adduct of trimethylolpropane (1 mol)): 20 parts Carbon black (BP800 manufactured by Cabot Corporation): 100 Parts dispersant (lecithin): 1 part lubricant (copper oleate): 1 part diluent (methyl ethyl ketone / cyclohexanone = 2/1): 200 parts diluent (toluene / MIBK): 150 parts

[0057]

[Table 1]

As a result of the above Table 1, in the polishing of the optical connector ferrule by the polishing bodies of Comparative Example 1 containing no nitrocellulose resin as a binder and Comparative Example 2 containing no abrasive, the light quantity transmission loss was 45 to 42 dB. In addition, the step difference at the tip has a large value of 20 to 25 nm. On the other hand, in the case of the present invention, the light quantity transmission loss is a good value of 50 dB and the step is also a small value, but the amount of nitrocellulose resin is particularly 20 to 40 parts in Examples 2 and 3. In this case, the difference in level is small, which is good.

<Examples 6 to 10> In the abrasive body of this example, a polishing coating solution prepared by blending with the following composition B and dispersing and adjusting with a sand grinder was applied to a polyester support having a thickness of 75 µm to a thickness of 1 µm. A bar coat was applied to form a polishing layer. In Examples 6 to 10, the compounding amount of the abrasive with respect to 100 parts by weight of the binder was changed.

The above-mentioned polishing body (polishing sheet) has a diameter of 140
It was punched into a disc shape of mm and attached to a rubber rotary table in the same manner as in the above-mentioned example, and while the rotary table was rotated at 100 rpm, the optical connector ferrule was brought into contact with the planetary motion while being ground for 50 seconds. As the supplied coolant liquid, an aqueous solution containing colloidal silica having a particle diameter of 0.05 μm was used.

Table 2 shows the measurement results of the compounding amount of the polishing agent and the surface roughness Ra of the polishing layer, the measurement result of the step, and the measurement result of the light quantity transmission loss in the polishing bodies according to Examples 6 to 10.

<Comparative Example 3> Table 2 also shows the measurement results of the abrasive body of Comparative Example 3. In this comparative example, the polishing layer does not contain an abrasive.

[Coating liquid composition: B] Abrasive (chromium oxide, particle size 0.2 μm): Z part Binder (nitrocellulose resin): 40 parts Binder (polyester polyurethane, sulfonic acid group 3 × 10 ⁻³ equivalent / g) , Epoxy group 2 × 10 ⁻⁵ equivalent / g): 30 parts Binder (polyisocyanate, TDI (3 mol) adduct of trimethylolpropane (1 mol)): 20 parts Carbon black (Conductex SC manufactured by Cabot): 100 parts Dispersant (oleic acid): 1 part Lubricant (butyl myristate): 1 part Diluent (methyl ethyl ketone / cyclohexanone = 2/1): 250 parts Diluent (xylene / MIBK / toluene = 1/1/1) : 250 copies

[0064]

[Table 2]

From the results shown in Table 2 above, in the abrasive body of Comparative Example 3 containing no abrasive, the level difference on the polished optical fiber surface was large, and the loss of transmitted light amount was increased. On the other hand, with the abrasives of Examples 6 to 10 of the present invention, good polishing characteristics were obtained, the level difference on the polished optical fiber surface was small, and the light quantity transmission loss was also reduced.

[0066]

Claims (4)

[Claims] 1. A polishing body used for polishing the tip of an optical connector ferrule having an optical fiber inserted and fixed in a ferrule hole into a convex spherical surface, wherein the flexible support comprises a polishing agent and a binder. And a center line average surface roughness Ra of the polishing layer is 0.
A polishing body for an ultra-low reflection optical connector ferrule having a diameter of 01 to 0.05 μm and using a cellulose resin as a binder. 2. The polishing body for an ultra-low reflection optical connector ferrule according to claim 1, wherein polishing is performed with a coolant liquid supplied to the surface of the polishing layer. 3. The polishing body for an ultra-low reflection optical connector ferrule according to claim 2, wherein the coolant contains polishing fine particles made of alumina or silica. 4. The polishing body for an ultra-low reflection optical connector ferrule according to claim 3, wherein the silica is colloidal silica.