JPH11277450A - Polishing body - Google Patents

Abstract

PROBLEM TO BE SOLVED: To polish while maintaining high polishing force without generating a stage difference while securing smoothness of a ferrule surface and an optical fiber surface by including a specified percentage or more of carboxymethyl nitrocellulose in the binder. SOLUTION: A polishing body has a polishing layer formed of the polishing agent and the binder including at least 50 % or more of carboxymethyl nitrocellulose in one surface of a flexible support. An undercoat layer is provided between the flexible support and the polishing layer at need, or a back layer is provided in a back surface of the support at need. Substituent degree of the nitro group of the carboxymethyl nitrocellulose is set at 1.6-2.2, and the water soluble characteristic is given to the carboxymethyl nitrocellulose. The polishing body is stuck to a rotary base of the elastic material such as rubber, and a tip of an optical connector ferrule is pushed for contact with this polishing body, and the rotary base is rotated, and the optical connector ferrule is moved for epicyclic movement for polishing.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polishing body for polishing an end face of an optical connector ferrule, and more particularly to a polishing body such as a polishing sheet and a polishing disk used for polishing a ceramic material such as quartz glass, optical glass, silica, alumina and zirconia. It is.

[0002]

2. Description of the Related Art For example, the end face of an optical connector ferrule in which an optical fiber is inserted into and fixed in a ferrule hole is polished using a polishing body or a polishing slurry. Are not necessarily sufficient.

As an example, as disclosed in Japanese Patent Application Laid-Open No. 3-81708, a constant 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 the resin film. There has been proposed a polishing method using a free-abrasive holding film in which a coolant liquid having a silica-based abrasive is supplied to a contact portion thereof while being slid and polished.

[0004]

However, it is useful to use nitrocellulose as a polishing body for an optical connector ferrule or the like as described above. This requires careful attention to production control.

In addition, the end face of the optical connector ferrule has:
Various materials including various ceramics such as glass materials, alumina, and zirconia are included, and they must be uniformly cut to prevent optical transmission loss. That is,
It has been very difficult to maintain the smoothness between the ferrule surface and the optical fiber surface and polish it so as not to cause a step between the ferrule surface and the optical fiber surface 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 due to the material difference, such as polishing the polishing body while holding the polishing body in an elastic state in order to polish the tip into a convex spherical surface, etc. For this reason, it is difficult to polish into a desired shape, and management of polishing conditions and the like are complicated.

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 the tip of an optical connector ferrule.

[0008]

In order to solve the above-mentioned problems, the polishing body of the present invention is characterized in that a polishing layer comprising fine abrasive powder and a binder is provided on a flexible support, wherein the binder comprises carboxymethyl nitrocellulose. It is characterized by containing 50% or more.

Further, the polishing body is suitable for polishing an end face of an optical connector ferrule. Further, the binder desirably contains carboxymethylnitrocellulose having a nitro group substitution degree of 1.6 to 2.2. The binder preferably comprises carboxymethyl nitrocellulose provided with water solubility.

[0010]

According to the present invention as described above, since the binder contains 50% or more of carboxymethylnitrocellulose, for example, the tip of the optical connector ferrule can be formed into a desired convex spherical surface, the ferrule surface and the optical fiber surface. Polishing can be performed while maintaining a high polishing force without generating a step while ensuring smoothness of the surface, the optical loss is reduced, the transmission efficiency is improved, and the polishing process can be easily performed.

In particular, by using carboxymethyl nitrocellulose as an aqueous nitrocellulose as a binder, the firing explosive property of the polishing layer coating solution before coating on a flexible support is small, and the contribution of nitrocellulose after coating is low. Since it is small, it is easy to handle, which is advantageous in production management.

[0012]

BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, embodiments of the polishing body of the present invention will be shown, and the present invention will be described in more detail.

The polishing body (polishing sheet) of this embodiment has a polishing layer made of a polishing agent and a binder containing at least 50% or more of carboxymethylnitrocellulose on one surface of a flexible support. Further, 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 carboxymethyl nitrocellulose is also called aqueous nitrified cotton, and has a structure in which a hydroxyl group of a cellulose skeleton is substituted with a specific amount of a carboxymethyl ether group and a nitrate ester group as shown in the following chemical formula. It is a molecular electrolyte. The carboxymethylnitrocellulose has a nitro group substitution degree of 1.6 to 2.
2, which is water-soluble. The weight average molecular weight is 20,000 to 50,000, the degree of substitution is 1.6 to 2.2 for nitrate ester, 0.4 to 1.0 for carboxymethyl ester, and 0.1 for hydroxyl group.
~ 1.0.

[0015]

Embedded image

In the polishing body, an end face of an optical connector ferrule formed by inserting and fixing an optical fiber of a glass material (for example, quartz) into a center hole of a pipe-shaped ferrule made of a ceramic material (for example, ZrO2) is made smooth without any step. It is suitable for polishing a convex spherical surface having a predetermined radius of curvature.

As an example of polishing the tip of an optical connector ferrule using the polished body according to the present invention, the polished body is attached to a rotating table made of an elastic material such as rubber, and the polished body is pressed into contact with the tip of the optical connector ferrule. Then, the rotating table is rotated, and the optical connector ferrule is caused to move in a planetary motion to be polished.

At this time, a dry type may be used, but a wet type is preferred. In the wet method, it is preferable to supply an aqueous solution of a coolant, and the coolant contains abrasive fine particles (silica, alumina, etc.).
May be included. In the case of silica, colloidal silica is preferable, and the particle diameter is 0.005 to 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.

The abrasive used in the polishing layer is generally a material having a polishing action or a polishing action, such as α-alumina, γ-alumina, α · γ-alumina, fused alumina,
Silicon carbide, chromium oxide, corundum, artificial diamond, diamond, α-iron oxide, silicon nitride, boron nitride,
Molybdenum carbide, boron carbide, tungsten carbide, titanium carbide, silica, zirconia, titanium oxide, cerium oxide, red iron oxide, garnet, and the like are mainly used. These abrasives have an average particle size of 0.1 to 50 μm.
A size of m is used. In the case of a polishing layer, a binder is used in an amount of 10 to 1000 parts by weight based on 100 parts by weight of the abrasive.

Specific examples of these abrasives include AKP1, AKP15, AKP20, AKP30, and AKP1, manufactured by Sumitomo Chemical Co., Ltd.
AKP50, AKP80, Hit50, Hit100 and the like. These are described in JP-B-52-2864.
No. 2, JP-B-49-39402, JP-A-63-988
No. 28, U.S. Pat. No. 3,687,725, U.S. Pat.
No. 807, U.S. Pat. No. 3,041,196, U.S. Pat.
No. 3,066, U.S. Pat. No. 3,630,910, U.S. Pat.
No. 33412, US Pat. No. 4,117,190, British Patent 1
No. 145,349, West German Patent No. 853211 and the like.

The binder used in the polishing layer of the present invention contains 50% by weight or more of carboxymethylnitrocellulose. In addition to this, conventionally known thermoplastic resins, thermosetting resins, reactive resins, and electronic resins A line-curable resin, an ultraviolet-curable resin, a visible light-curable resin, or a mixture thereof is used.

Other thermoplastic resins have a softening temperature of 200 ° C. or less and an average molecular weight of 10,000 to 30,000.
0, having a polymerization degree of about 10 to 2000, and more preferably about 50 to 800. Examples thereof include vinyl chloride vinyl acetate copolymer, vinyl chloride copolymer, vinyl chloride vinyl acetate vinyl alcohol copolymer, and vinyl chloride. Vinyl alcohol copolymer, vinyl chloride vinylidene chloride copolymer,
Vinyl acrylonitrile chloride copolymer, acrylate acrylonitrile copolymer, acrylate vinylidene chloride copolymer, acrylate styrene copolymer, methacrylate acrylonitrile copolymer, methacrylate vinylidene chloride copolymer, methacryl Acid ester styrene copolymer, urethane elastomer, nylon-silicone resin, nitrocellulose-polyamide resin, polyfuccavinyl, vinylidene chloride acrylonitrile copolymer, butadiene acrylonitrile copolymer, polyamide resin, polyvinyl butyral,
Cellulose derivatives (cellulose acetate butyrate,
Cellulose diacetate, cellulose triacetate, cellulose propionate, nitrocellulose, ethylcellulose, methylcellulose, propylcellulose, methylethylcellulose, carboxymethylcellulose, acetylcellulose, etc.), styrene butadiene copolymer, polyester resin, polycarbonate resin, chlorovinyl ether acrylate Various synthetic rubber-based thermoplastic resins, such as copolymers, amino resins, and polyamide resins, and mixtures thereof are used. Examples of these resins are described in JP-B-37-6877 and JP-B-39-1.
No. 2528, Japanese Patent Publication No. 39-19282, Japanese Patent Publication No. 40-
No. 5349, Japanese Patent Publication No. 40-20907, Japanese Patent Publication No. 41-
9463, JP-B-41-14059, JP-B-41-140-
No. 16985, JP-B-42-6428, JP-B-42-428
No. 11621, JP-B-43-4623, JP-B-43-
No. 15206, JP-B-44-2889, JP-B-44-
17947, JP-B-44-18232, JP-B-45
No. 14020, No. 45-14500, No. 4
7-18573, JP-B-47-22063, JP-B-47-22264, JP-B-47-22068, JP-B-47-22069, JP-B-47-22070, JP-B-47-27886, and JP-A-47-27886. 57-133521
JP-A-58-137133, JP-A-58-166
No. 533, JP-A-58-222433, JP-A-59-222.
No. 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 solution, and becomes infinite by a reaction such as condensation and addition by heating and humidifying after coating and drying. Is suitable. Among these resins, those which 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 resin Mixture of polymers, mixture of methacrylate copolymer and diisocyanate prepolymer, mixture of polyester polyol and polyisocyanate, urea formaldehyde resin, mixture of low molecular weight glycol / high molecular weight diol / triphenylmethane triisocyanate, polyamine resin, polyimine Resins and mixtures thereof. Examples of these resins are described in JP-B-39-8.
No. 103, Japanese Patent Publication No. 40-9779, Japanese Patent Publication No. 41-71
No. 92, JP-B-41-8016, JP-B-41-142
No. 75, JP-B-42-18179, JP-B-43-12
No. 081, Japanese Patent Publication No. 44-28023, Japanese Patent Publication No. 45-1
No. 4501, No. 45-24902, No. 46-
No. 13103, JP-B-47-2265, JP-B-47
-22066, JP-B-47-22067, JP-B-4
No. 7-22072, JP-B-47-22073, JP-B-47-28045, JP-B-47-28048, JP-B-47-28922 and the like.

These thermoplastic resins, thermosetting resins, and reactive resins have carboxylic acid (COOM), sulfinic acid, sulfenic acid, sulfonic acid (SO ₃ M), and phosphoric acid (SOOM) as functional groups other than the main functional groups. PO (OM) (OM)),
Acid groups such as phosphonic acid, sulfuric acid (OSO ₃ M) and ester groups thereof (M is H, alkali metal, alkaline earth metal, hydrocarbon group), amino acids, aminosulfonic acids,
Sulfuric or phosphoric acid esters of amino alcohols, amphoteric groups such as alkyl betaine type, amino groups, imino groups, imide groups, amide groups, etc .; hydroxyl groups, alkoxyl groups, thiol groups, alkylthio groups, halogen groups (F, Cl , B
r, I), usually one or more but not more than six kinds of silyl group, siloxane group, epoxy group, isocyanato group, cyano group, nitrile group, oxo group, acryl group and phosphine group, and each functional group is 1 to 1 g of resin. × 10 ^-6 eq to 1 × 10
^-2 eq is preferred.

Examples of the polyisocyanate 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, and isophorone diisocyanate. , Triphenylmethane triisocyanate, isophorone diisocyanate, etc., products of said isocyanates and polyalcohols, polyisocyanates of 2-10 mer produced by condensation of isocyanates, and products of polyisocyanates and polyurethanes Those whose terminal functional groups are isocyanates can be used.

The average molecular weight of these polyisocyanates is preferably from 100 to 20,000. Commercially available trade names of these polyisocyanates include Coronate L, Coronate HL, Coronate 2030, Coronate 2031, Millionate MR, and Millionate MT.
L (manufactured by Nippon Polyurethane), Takenate D-102,
Takenate D-110N, Takenate D-200, Takenate D-202, Takenate 300S, Takenate 5
00 (manufactured by Takeda Pharmaceutical Co., Ltd.), Sumidur T-80, Sumidur 44S, Sumidur PF, Sumidur L, Sumidur 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 Co., Ltd.), and the like. Can be used in combination of two or more utilizing the difference between the two. In order to accelerate the curing reaction, a hydroxyl group (butanediol, hexanediol, having a molecular weight of 1,000 to 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. It is desirable that these compounds having a hydroxyl group or an amino group are polyfunctional.
These polyisocyanates are preferably used in an amount of 2 to 70 parts by weight, more preferably 5 to 50 parts by weight, per 100 parts by weight of the total amount of the binder resin and the polyisocyanate in both the polishing layer and the back layer. Examples of these are disclosed in JP-A-60-131622 and JP-A-61-74138.

[0027] 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. The mixing ratio of the powder 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 powdery lubricant used in the polishing layer of the present invention includes graphite, molybdenum disulfide, boron nitride, graphite fluoride, calcium carbonate, barium sulfate, silicon oxide, titanium oxide, zinc oxide, tin oxide, and the like. Inorganic fine powder such as tungsten disulfide, acrylic styrene resin fine powder, benzoguanamine resin fine powder, melamine resin fine powder,
Resin fine powders such as polyolefin resin fine powder, polyester resin fine powder, polyamide resin fine powder, polyimide resin fine powder, and polyfucker ethylene resin fine powder.

As the organic compound-based lubricant, silicone oil (dialkyl polysiloxane, dialkoxy polysiloxane, phenyl polysiloxane, fluoroalkyl polysiloxane (KF96, KF69 manufactured by Shin-Etsu Chemical Co., Ltd.)
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 Fatty acid, perfluoro fatty acid ester, perfluoroalkyl sulfate, perfluoroalkyl sulfonate, perfluoroalkyl benzene sulfonate, perfluoroalkyl phosphate, and other compounds containing fluorine or silicon, alkyl sulfate, alkyl sulfonate , Alkyl phosphonic acid triesters,
Organic acids and organic acid ester compounds such as alkyl phosphonic acid monoesters, alkyl phosphonic acid diesters, alkyl phosphate esters, succinate esters, etc .; triazaindolizine, tetraazaindene, benzotriazole, benzotriazine, benzodiazole, EDTA, etc. Heterocyclic compound 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
Fatty acid esters of monohydric to hexahydric alcohols having a total of 11 to 70 carbon atoms in total with at least one monobasic fatty acid and the number of carbon atoms of the fatty acid; a fatty acid or fatty acid amide having 8 to 40 carbon atoms , Fatty acid alkylamides and aliphatic 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, alkyl stearic acid, 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:
So-called lubricating oil additives can be used alone or in combination. Antioxidants (alkylphenol, benzotriazine, tetraazaindene,
Sulfamide, guanidine, nucleic acid, pyridine, amine,
Metal chelating agents such as hydroquinone and EDTA), 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.),
There are cleaning 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.
-24041, JP-B-48-18482, JP-B-4
No. 4-18221, JP-B-47-28043, JP-B-57-56132, JP-A-59-8136, JP-A-59-8139, JP-A-61-85621, U.S. Pat. No. 3,423,233, U.S. Pat. No. 3470021, US Pat. No. 3,492,235, US Pat. No. 3,497,411, US Pat. No. 3,230,086, US Pat. No. 3,625,760,
U.S. Pat. No. 3,630,772, U.S. Pat. No. 3,634,253
No. 3,642,539, US Pat. No. 3,687,772.
5, U.S. Pat. No. 4,350,031, U.S. Pat.
No. 64, U.S. Pat. No. 4,552,794, IBM Technical Disclosure Bulletin (IBM Tech)
Nical Disclosure Bulleti
n) Vol. 9, No7, p779 (1966 December 12)
Mon), Electronic (ELEKTRONIK) 196
1 year No12, p380, "Chemical Handbook (Application)" p9
54-967, published by Maruzensha in 1980.

As the dispersant and dispersing aid of the abrasive used in the present invention, 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 to 40 fatty acids (R ₁ COOH, R ₁ has ₁ to 39 carbon atoms)
Alkyl groups, phenyl groups, aralkyl groups), alkali metals (Li, Na, K, NH ₄ ^+, etc.) or alkaline earth metals (Mg, Ca, Ba, etc.), Cu,
Metal soap (copper oleate) made of Pb or the like, fatty acid amide, lecithin (soybean oil lecithin) and the like are used. 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 compounds and the like can also be used. In addition, polyethylene glycol, polyethylene oxide, sulfosuccinic acid, metal salts of sulfosuccinic acid, sulfosuccinate, and the like can also be used. One or more of these dispersants are usually used, and one kind of the dispersant is added in an amount of 0.005 to 20 parts by weight based on 100 parts by weight of the binder. Regarding the method of using these dispersants, the dispersants may be previously adhered to the surface of the abrasive or the non-abrasive fine powder, or may be added during dispersion.
Such a product is disclosed, for example, in 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.

The fungicides used in the present invention include 2- (4
-Thiazolyl) -benzimidazole, N- (fluorodichloromethylthio) -phthalimide, 10.10'-
Oxybisphenoxalcin, 2.4.5.5.6 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).

The above-mentioned polishing layer may contain carbon black as an antistatic agent. For example, furnace black for rubber, thermal for rubber, black for color, acetylene black and the like can be used. Its specific surface area is 5-5
00m ² / g, DBP oil absorption 10-400ml / 10
It is preferable that 0 g, the pH is 2 to 10, the water content is 0.1 to 10%, and the tap density is 0.1 to 1 g / cm ² . Specific examples of this carbon black include: BLACKPEARLS 2000, 1300, manufactured by Cabot Corporation.
1000, 900, 800, 700, manufactured by Mitsubishi Kasei Kogyo: 650B, 950B, 3250B, 850, 90
0,960,980,1000,2300,2400,
2600 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, ester amides, 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 group, phosphonate ester, phosphate group; amino acids; aminosulfonic 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. 2,676,975, 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
41413, 3444254, 3475174
No. 3,545,974, West German Patent Publication (OLS) 19
No. 42665, British Patent Nos. 1077317, 1198
No. 450, Ryohei Oda et al., "Synthesis of Surfactants and Their Applications" (Maki Shoten, 1972 edition); W. "Surfes Active Agents" 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"
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 to 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. 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 Alcohols such as, isobutyl alcohol, isopropyl alcohol, 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; N / N-dimethylformaldehyde , Hexane and the like can be used. These solvents are generally 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 in the polishing coating solution.
It is used in an amount of 50 to 20,000 parts by weight based on 00 parts by weight. The preferred solid content of the polishing coating solution is 5 to 60% by weight. Instead of an organic solvent, an aqueous solvent (water, alcohol,
Acetone, etc.) can also be used.

The polishing layer is formed by dissolving in an organic solvent any combination of the above-mentioned compositions and the like, and applying and drying the solution on a support as a coating solution. This support is flexible and has a thickness of 50
About 300 μm. Examples of the material 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, and polysulfone. In addition to the above plastics, 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. Regarding these supports, see, for example, West German Patent 3,338,854A, JP-A-59-5959.
No. 116926, JP-A-61-129731, U.S. Pat. No. 4,388,368; Yukio Mitsuishi, Textile and Industry, vol. 31, p. 50-55, 1975, etc. The center line average surface roughness Ra of these supports is 0.001-5.
0 μm is preferred. In addition, the Young's modulus (F5
Value) is 2 to 30 kg in both the width and longitudinal directions depending on the purpose.
/ Mm ² (1 kg / m ² = 9.8 Pa).

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. For preparation of the polishing coating solution, a usual kneading machine, 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 disperser, a high-speed stone mill, and a high-speed Impact mill, disperser, kneader, high-speed mixer, ribbon blender, co-kneader, intensive mixer,
Tumblers, blenders, dispersers, homogenizers, single screw extruders, twin screw extruders, ultrasonic dispersers, and the like can be used. Usually, dispersing / kneading is provided with a plurality of these dispersing / kneading machines,
Process continuously. For more information on kneading and dispersing technology,
T. C. PATTON (T.C.Patton) "P
aint Flow and Pigment Dis
version "(Paint Flow and Pigment Dispersion), 1964, John Wil
ey & Sons (John Wiley and Sons)) and Shinichi Tanaka, Industrial Materials, Vol. 25, 37 (1
977) and the cited reference of the book.
In order to efficiently promote dispersion and kneading as an auxiliary material for these dispersion and kneading, the equivalent diameter of the sphere is 10 cmφ to 0.05 mmφ.
Steel balls, steel beads, ceramic beads, glass beads, and organic polymer beads having the following diameters can be used. 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, a polishing coating solution can be prepared by kneading and dispersing according to the method described in the above book or the cited document of the book.

As a method of applying the above-mentioned coating liquid for a polishing layer on a support, the viscosity of the coating liquid is adjusted to 1 to 20,000 centistokes (25 ° C.), and an air doctor coater, a blade coater, an air knife coater, and a squeeze 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., and other methods are available. 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). The order of application of these coating liquids can be arbitrarily selected, and a 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
JP-1235232, JP-B-62-37451, JP-A-59-142741 and JP-A-59-1.
No. 65239, and the like.

By such a method, about 1 to about
If necessary, the polishing liquid applied at about 200 μm is immediately subjected to drying treatment at 30 to 160 ° C. in multiple stages, and then the formed polishing layer is dried to a thickness of 0.05 to 10 μm. The conveying speed of the support at this time is usually 10 m / min to 900
m / min, and drying temperature is 20 ° C in multiple drying zones.
~ 130 ° C and the amount of residual solvent in the coating film is 0.1 ~ 4
0 mg / m ² . Further, if necessary, the surface of the polishing layer or the backing layer is subjected to a surface smoothing process so that the center line average surface roughness of the polishing layer or the backing layer is 0.001 to 0.3 μm (cutoff 0.25 mm) and cut into a desired shape. Is manufactured. These production methods include powder pretreatment / surface treatment, kneading / dispersion, coating / drying, smoothing treatment, heat treatment, EB
It is desirable that the steps of treatment, surface polishing, cutting, and winding are performed continuously.

The polished body thus produced is cut or punched into a predetermined shape. It is desirable to burnish and / or clean the abrasive body in an earlier step. The burnisher uses a hard material such as a sapphire blade, a razor blade, a cemented carbide blade, a diamond blade, or a ceramic blade to scrape off 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 need to be a blade in particular, and may be a shape such as a square shape, a round shape, or a wheel (these materials may be provided around a rotating cylindrical shape). The cleaning of the abrasive body is performed by wiping the surface of the abrasive body with a nonwoven fabric or the like in order to remove dirt or excess lubricant on the surface of the abrasive body. Examples of such wiping materials include various types of Vilene manufactured by Nippon Vilene, Toraysee, Exeine, manufactured by Toray.
Trade name: Kimwipe, various polishing tapes made by Fuji Photo Film, and nonwoven fabrics: nylon nonwoven fabric, polyester nonwoven fabric, rayon nonwoven fabric, acrylonitrile nonwoven fabric,
Tissue paper, such as a blended nonwoven fabric, can be used.
These are, for example, JP-B-46-39309 and JP-B-58
No. 46768, JP-A-56-90429, Japanese Patent Publication No. 5
No. 8-46767, JP-A-63-259830, JP-A-1-201824 and the like.

The abrasive, binder and binder used in the present invention
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 of a polishing body described in JP-B-56-26890 and the like.

[0046]

EXAMPLES Examples and comparative examples of the present invention will be shown below, and their polishing characteristics will be evaluated. In the examples, “parts” means “parts by weight”.

<Examples 1 to 5> A polishing body of the present example was prepared by uniformly kneading and dispersing the following composition A and adjusting the viscosity of the polishing composition.
A polishing layer was formed by applying and drying a bar coat to a thickness of 2 to 50 μm on a support made of polyethylene terephthalate having a thickness of 75 μm to obtain a sample X. Example 1
In No. 5, the coating thickness of the polishing layer was changed as shown in Table 1 below.

The above-mentioned abrasive body (abrasive sheet) was prepared by
mm, and affixed on a rubber turntable. The turntable was rotated at 100 rpm, and the optical connector ferrule was made to perform planetary motion on the ferrule to bring the tip into contact with the polishing layer to perform polishing for 30 seconds. Was. As the supplied coolant, a silica slurry containing colloidal silica having a particle diameter of 10 nm was used.

Table 1 shows the thickness of the polishing layer applied to the above-mentioned polished body, the measurement results of the step between the ferrule surface and the optical fiber surface, and the measurement results of the optical loss of the polished optical connector ferrule. The light loss (dB) is a value obtained by measuring a loss amount of a transmitted light amount caused by reflection on a polished surface of an optical fiber.
The smoothness and the like of the surface can be evaluated. The larger the dB value, the smaller the transmission loss and the better the transmission state.

<Comparative Examples 1-4> Table 1 also shows the test results of Comparative Examples 1-4. In this comparative example, polishing bodies having different compositions were used, and in each case, the binder of the polishing layer did not contain carboxymethylnitrocellulose.

[Coating liquid composition: A] Abrasive (alumina: WA8000 manufactured by Fujimi Abrasives) 30 parts Binder (water-soluble carboxymethylnitrocellulose: nitrification degree 11.1%, substitution degree 2) 10 parts Binder (urethane emulsion HW140) Dainippon Ink Co., Ltd.) 20 parts Solvent (alcohol aqueous solution) 60 parts

[0052]

[Table 1]

As a result of the above Table 1, in Examples 1 to 5 of the present invention, the light loss is as good as 59 to 60 dB, and the step is as small as 3 to 5 μm. On the other hand, when the optical connector ferrule was polished with the polished bodies of Comparative Examples 1, 2, and 4 containing no carboxymethylnitrocellulose as a binder, the light loss was 48-5.
It is 3 dB, and the step at the tip is a large value of 6 to 25 nm. In Comparative Example 3, a cellulose film containing no abrasive was polished using an abrasive-containing slurry. The step was as small as 2 nm, but the light loss was 55 dB, which was higher than that of the embodiment of the present invention. Efficiency is low.

Claims (4)

[Claims] 1. A polishing body having a polishing layer comprising fine abrasive powder and a binder provided on a flexible support, wherein the binder contains 50% or more of carboxymethylnitrocellulose. 2. The polishing body according to claim 1, wherein the polishing body is for polishing an end face of an optical connector ferrule. 3. The polishing body according to claim 1, wherein the binder contains carboxymethylnitrocellulose having a nitro group substitution degree of 1.6 to 2.2. 4. The polishing body according to claim 1, wherein the binder contains carboxymethylnitrocellulose provided with water solubility.