US20170175021A1 - Steel wire rod having lubricating coating film that has excellent corrosion resistance and workability - Google Patents

Steel wire rod having lubricating coating film that has excellent corrosion resistance and workability Download PDF

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Publication number
US20170175021A1
US20170175021A1 US15/129,321 US201515129321A US2017175021A1 US 20170175021 A1 US20170175021 A1 US 20170175021A1 US 201515129321 A US201515129321 A US 201515129321A US 2017175021 A1 US2017175021 A1 US 2017175021A1
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United States
Prior art keywords
water
coating film
soluble
lubricating coating
steel wire
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Abandoned
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US15/129,321
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English (en)
Inventor
Keita Shiihashi
Kasumi Yanagisawa
Hirotaka Ito
Takahiro Ozawa
Shinobu Komiyama
Tsuyoshi Hatakeyama
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kobe Steel Ltd
Nihon Parkerizing Co Ltd
Original Assignee
Kobe Steel Ltd
Nihon Parkerizing Co Ltd
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Filing date
Publication date
Application filed by Kobe Steel Ltd, Nihon Parkerizing Co Ltd filed Critical Kobe Steel Ltd
Assigned to NIHON PARKERIZING CO., LTD., KABUSHIKI KAISHA KOBE SEIKO SHO (KOBE STEEL, LTD.) reassignment NIHON PARKERIZING CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HATAKEYAMA, TSUYOSHI, KOMIYAMA, SHINOBU, YANAGISAWA, KASUMI, ITO, HIROTAKA, OZAWA, TAKAHIRO, SHIIHASHI, KEITA
Publication of US20170175021A1 publication Critical patent/US20170175021A1/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
    • C10M103/06—Metal compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C9/00—Cooling, heating or lubricating drawing material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C9/00—Cooling, heating or lubricating drawing material
    • B21C9/02—Selection of compositions therefor
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/02—Carbon; Graphite
    • C—CHEMISTRY; METALLURGY
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    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/10—Metal oxides, hydroxides, carbonates or bicarbonates
    • C—CHEMISTRY; METALLURGY
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    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/22—Compounds containing sulfur, selenium or tellurium
    • C—CHEMISTRY; METALLURGY
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    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/26—Compounds containing silicon or boron, e.g. silica, sand
    • C—CHEMISTRY; METALLURGY
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    • C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/26—Carboxylic acids; Salts thereof
    • C10M129/28—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
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    • C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
    • C10M129/26—Carboxylic acids; Salts thereof
    • C10M129/28—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M129/38—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms
    • C10M129/40—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms monocarboxylic
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    • C10M133/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing nitrogen having a carbon chain of less than 30 atoms
    • C10M133/16—Amides; Imides
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    • C10M145/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M145/04—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to an alcohol, aldehyde, ketonic, ether, ketal or acetal radical
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    • C10M145/02—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M145/10—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate
    • C10M145/12—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate monocarboxylic
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    • C10M145/40—Polysaccharides, e.g. cellulose
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    • C10M147/02—Monomer containing carbon, hydrogen and halogen only
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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    • C10N2010/02—Groups 1 or 11
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/04—Groups 2 or 12
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/12—Groups 6 or 16
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/12—Inhibition of corrosion, e.g. anti-rust agents or anti-corrosives
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/24—Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/32—Wires, ropes or cables lubricants
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/015—Dispersions of solid lubricants
    • C10N2050/02—Dispersions of solid lubricants dissolved or suspended in a carrier which subsequently evaporates to leave a lubricant coating

Definitions

  • the present invention relates to a steel wire rod having a lubricating coating film containing no phosphorus on a surface.
  • a surface of a metal material is coated in advance with a solid coating film, for example, an inorganic coating film such as a borate coating film or a phosphate crystal coating film, which has sufficient coating film strength and exists at an interface between a die and a workpiece and is therefore less likely to cause lubricating coating film disruption even under high surface pressure, thus making it possible to avoid direct contact between metals.
  • a composite coating film composed of a zinc phosphate coating film and a soap layer hereinafter sometimes referred to as a chemical conversion coating film has widely been employed because of having high workability and corrosion resistance.
  • Patent Document 1 discloses an aqueous lubricating coating agent for plastic working of a metal material, which is a composition comprising an aqueous inorganic salt (A) and a wax (B) dissolved or dispersed in water, wherein a solid component weight ratio (B)/(A) is in a range of 0.3 to 1.5; and a coating film forming method thereof.
  • Patent Document 2 discloses an aqueous lubricating coating agent for plastic working of a metal material, comprising an alkali metal borate (A), wherein the alkali metal borate (A) contains lithium borate, a molar ratio of lithium to the entire alkali metal in the alkali metal borate (A) is in a range of 0.1 to 1.0, and also a molar ratio (B/M) of boric acid B to an alkali metal M of the alkali metal borate (A) is in a range of 1.5 to 4.0; and a coating film forming method thereof. It is considered that this technology suppresses crystallization of a coating film caused by moisture absorption of the coating film, thus enabling formation of a coating film having not only workability but also high corrosion resistance.
  • Patent Document 3 discloses a water-soluble lubricant for non-phosphorus based plastic working, comprising an inorganic solid lubricant as a component A, a wax as a component B, and a water-soluble inorganic metal salt as a component C, wherein a solid component mass ratio of the component A to the component B (component A/component B) is in a range of 0.1 to 5, and a solid component mass ratio of the component C to the total amount of the component A, the component B, and the component C (component C/(component A+component B+component C)) is in a range of 1 to 30°. It is considered that this technology is directed to a lubricant containing no phosphorus and enables realization of corrosion resistance equal to that of a chemical conversion coating film.
  • Patent Document 4 discloses an aqueous lubricating coating agent comprising an aqueous inorganic salt (A), at least one lubricant (B) selected from molybdenum disulfide and graphite, and a wax (C), these components being dissolved or dispersed in water, wherein (B)/(A) is in a range of 1.0 to 5.0 in terms of a solid component weight ratio, and (C)/(A) is in a range of 0.1 to 1.0 in terms of a solid component weight ratio; and a coating film forming method thereof. It is considered that this technology enables realization of high workability having the same level as that of a chemical conversion coating film by mixing a conventional aqueous lubricating coating agent with molybdenum disulfide or graphite.
  • Patent Document 5 discloses a coating film forming agent comprising a silicate (A), a polycarboxylate (B), a hydrophilic polymer and/or a hydrophilic organic lamellar structure (C), and a molybdate and/or a tungstate (D), a mass ratio of each component being a predetermined ratio.
  • the aqueous inorganic salt is an essential component in the solid coating film of the aqueous lubricating coating agent.
  • the lubricating coating film composed of the aqueous inorganic salt has sufficient coating film strength and, as mentioned above, the lubricating coating film exists at an interface between a die and a workpiece and is therefore less likely to cause lubricating coating film disruption even under high surface pressure, thus making it possible to avoid direct contact between metals.
  • aqueous lubricating coating agent it is possible to maintain a satisfactory lubricated state during plastic working by using a solid coating film composed of an aqueous inorganic salt or a water-soluble resin in combination with an appropriate lubricant capable of reducing a friction coefficient.
  • An aqueous inorganic salt of a water-soluble component is in a state of being dissolved in water in a lubricating treatment solution and, when a lubricant is applied on a surface of a metal material and then dried, water as a solvent is vaporized to form a lubricating coating film.
  • the aqueous inorganic salt is precipitated as a solid substance on the surface of the metal material to form a solid coating film.
  • the solid coating film thus formed has a coating film strength capable of enduring plastic working, and exhibits satisfactory lubricity during plastic working by mixing with an appropriate lubricant capable of reducing a friction coefficient.
  • Patent Document 1 WO 02/012420 A
  • Patent Document 2 JP 2011-246684 A
  • Patent Document 3 JP 2013-209625 A
  • Patent Document 4 WO 02/012419 A
  • Patent Document 5 JP 2002-363593 A
  • the aqueous lubricating coating film mentioned in Patent Document 3 exhibited corrosion resistance, which is equal to or better than that of the chemical conversion coating film, in a corrosion resistance test in a laboratory in which rusting is accelerated using a thermo-hygrostat.
  • the lubricating coating film is actually used in the environment where dusts and powders, and mists of a picking agent are adhesible. In such severe environment, corrosion resistance is actually inferior as compared with the chemical conversion coating film.
  • Examples of the aqueous inorganic salt capable of obtaining comparatively high corrosion resistance include an alkali metal salt of a silicate (hereinafter sometimes referred to as a silicate) and an alkali metal salt and/or an ammonium salt of a tungstate (hereinafter sometimes referred to as a tungstate). These aqueous inorganic salts are also mentioned in Patent Document 1, Patent Document 4, and Patent Document 5. However, they are far inferior in practical corrosion resistance as compared with the chemical conversion coating film.
  • the water-soluble silicate has a property that is less likely to transmit moisture among the water-soluble aqueous inorganic salts and also has very high adhesion to a material. Because of this property, it is a material that can exhibit comparatively high corrosion resistance, but not as much as the chemical conversion coating film. This is because the water-soluble silicate is crosslinked to from a network structure in a coating film formation process in which water as a solvent of a lubricant is vaporized. However, because of this network structure, the coating film of the water-soluble silicate is too brittle as a lubricating coating film. Therefore, when a base material is worked, it is sometimes impossible to sufficiently conform because of cracks of the coating film.
  • Too high adhesion due to the network structure may cause insufficient film removal, thus resulting in various defects in the subsequent step.
  • inclusion of a coating film component may cause not only contamination of a plating solution, but also poor plating in the portion where the coating film component remains.
  • the water-soluble tungstate is less likely to absorb moisture from external air when a coating film is formed. This is because granular crystals are formed when the water-soluble tungstate forms a coating film. Further, the water-soluble tungstate has a property that forms a passive coating film having a self-repair function on a surface of a steel material, and use of the water-soluble tungstate as the coating film component enables expectation of formation of a coating film having high corrosion resistance. Because of its high water solubility, it is possible to easily perform film removal with an aqueous solution. However, the water-soluble tungstate is crystalline and is therefore inferior in adhesion to a material and cannot form a uniform coating film, thus failing to obtain corrosion resistance and workability as expected. For example, it is possible to enhance adhesion and uniformity of a coating film by adding a synthetic resin component in a lubricant, but the corrosion resistance is drastically inferior as compared with a chemical conversion coating film.
  • Both of the aqueous lubricating coating agents containing an aqueous water-soluble inorganic salt mentioned in Patent Documents 1 to 3 were inferior in workability as compared with a chemical conversion coating film. This tendency is particularly notable in severe working wherein a surface area expansion ratio becomes at least several tens of times (hereinafter sometimes referred to as severe working), thus causing insufficient deformation of a material, decrease in die life, occurrence of seizure, and the like.
  • Patent Document 5 a coating film treatment agent containing a silicate (A) as a main component and containing excessively large amount of an anti-corrosive agent (D) is inferior in lubricity since seizure occurs under high extrusion load. Therefore, it becomes difficult to perform stable operation, thus failing to obtain sufficient long-term rust prevention property.
  • the aqueous lubricating coating agent could not form a coating film having both of high corrosion resistance over a long term of about two or more months and workability during severe working, that are comparable to those of a chemical conversion coating film, even under service environment. If a silicate is included in the aqueous lubricating coating agent, there may arise a problem such as insufficient film removal.
  • a steel wire rod including a lubricating coating film, which can reconcile workabilities such as wire drawability, spike property, ball ironing property and film removability, and corrosion resistance such as long-term rust prevention property.
  • the inventors of the present invention have intensively been studied so as to solve the above problems and found that it is possible to obtain high corrosion resistance and workability as well as sufficient adhesion and film removability that have never been achieved by each component alone, by adjustment of a ratio of a silicate to a tungstate are adjusted to a certain specific ratio, namely, adjustment of a mass ratio of water-soluble tungstate/water-soluble silicate to a predetermined ratio to form a composited lubricating coating film, and thus the present invention has been completed.
  • the present invention was structured in the following manner so as to solve the above problems.
  • the gist of the present invention lies in a steel wire rod including a lubricating coating film on a surface, wherein the lubricating coating film contains a water-soluble silicate and a water-soluble tungstate, a mass ratio of water-soluble tungstate/water-soluble silicate being in a range of 0.7 to 10, and contains no phosphorus.
  • the lubricating coating film is preferably formed using a composition prepared by mixing a water-soluble silicate and a water-soluble tungstate so as to adjust a mass ratio of water-soluble tungstate/water-soluble silicate in the lubricating coating film in a range of 0.7 to 10.
  • the lubricating coating film preferably contains a resin, and a mass ratio of resin/(water-soluble silicate+water-soluble tungstate) is preferably in a range of 0.01 to 1.5.
  • the resin is preferably at least one selected from a vinyl resin, an acrylic resin, an epoxy resin, a urethane resin, a phenol resin, a cellulose derivative, a polymaleic acid and a polyester resin.
  • the lubricating coating film preferably contains a lubricant, and a mass ratio of lubricant/(water-soluble silicate+water-soluble tungstate) is preferably in a range of 0.01 to 1.5.
  • the lubricant is preferably at least one selected from wax, polytetrafluoroethylene, fatty acid soap, fatty acid metal soap, fatty acid amide, molybdenum disulfide, tungsten disulfide, graphite and melamine cyanurate.
  • the mass of the coating film per unit area of the lubricating coating film is preferably in a range of 1.0 to 20 g/m 2 .
  • a lubricating coating film is structured in the manner mentioned above, thus obtaining a steel wire rod that has excellent workabilities such as wire drawability, spike property, ball ironing property and film removability, and corrosion resistance such as long-term rust prevention property.
  • the lubricating coating film in the present invention is far better than a conventional aqueous lubricating coating film in that all of these performances are equal to or better than those of steel wire rods having a chemical conversion coating film.
  • FIG. 1 shows evaluation criteria for seizure when ball ironing property is evaluated.
  • the present invention is directed to a steel wire rod including a lubricating coating film on a surface, wherein the lubricating coating film contains a water-soluble silicate and a water-soluble tungstate, a mass ratio of water-soluble tungstate/water-soluble silicate being in a range of 0.7 to 10, and contains no phosphorus.
  • a steel used in the steel wire rod also includes a carbon steel, an alloy steel, a special steel, and the like.
  • the steel wire rod generally refers to those obtained by forming a steel into a wire rod through hot working.
  • the steel wire is included in the steel wire rod of the present invention.
  • the steel wire refers to those obtained by further subjecting a steel wire rod to a working treatment, such as those obtained by drawing a steel wire rod into a wire having a specified size (wire diameter, circularity, etc.) and those obtained by subjecting a steel wire rod or a steel wire drawn into a wire to a plating treatment.
  • the steel wire rod of the present invention is not particularly limited as long as it is excellent in corrosion resistance and workability because of having the below-mentioned lubricating coating film, and a film, namely, an undercoating film may be further formed between a surface of the steel wire rod and the lubricating coating film. Both of these films may be a single layer, or a layer composed of two or more layers.
  • the lubricating coating film and the undercoating film contain no phosphorus, and a lubricating coating agent used for formation of the film does not contain a component containing phosphorus.
  • a component containing phosphorus is inevitably included in a coating film of a surface of the steel wire rod in the operation process. Namely, even if phosphorus as inevitable impurities may cause contamination in the actual operation, there is little possibility that phosphorus causes brittle fracture of a steel wire rod when the content of phosphorus is about 1% by mass or less, and thus it is possible to consider that phosphorizing does not occur.
  • the steel wire rod of the present invention to have a lubricating coating film on a surface, the lubricating coating film containing a water-soluble silicate and a water-soluble tungstate, and a mass ratio of water-soluble tungstate/water-soluble silicate being in a range of 0.7 to 10.
  • a lubricating coating film having high corrosion resistance and workability as well as sufficient adhesion and film removability that have never been achieved by the water-soluble silicate or the water-soluble tungstate alone, or the other aqueous inorganic salt.
  • the below-mentioned water-soluble silicate and water-soluble tungstate are composited to form a lubricating coating film, the water-soluble tungstate is incorporated into a network structure formed of the water-soluble silicate.
  • drawbacks of the water-soluble tungstate depend heavily on formation of a crystalline coating film and it becomes possible for the water-soluble tungstate to exist uniformly and finely by incorporating into the network structure of the water-soluble silicate. Whereby, it is possible to reconcile a property of being less likely to transmit moisture of the water-soluble silicate and a passive film having a self-repair function of the water-soluble tungstate, leading to a remarkable improvement in corrosion resistance.
  • Examples of the influence of the water-soluble tungstate on the water-soluble silicate include an improvement in workability and film removability.
  • the water-soluble silicate is inferior in workability and film removability since a firm continuous film is formed by polymerization of the water-soluble silicate.
  • the composited water-soluble tungstate exists in the network structure of the water-soluble silicate, whereby, formation of a firm network structure is appropriately suppressed, thus enabling an improvement in workability and film removability.
  • a ratio of the amount of the water-soluble tungstate to that of the water-soluble silicate is important.
  • a mass ratio of water-soluble tungstate/water-soluble silicate in the lubricating coating film is 0.7 or more, preferably 0.9 or more, and more preferably 1.1 or more.
  • the mass ratio is 10 or less, preferably 6.0 or less, and more preferably 3.0 or less. If the mass ratio of water-soluble tungstate/water-soluble silicate is less than 0.7, the obtained film can achieve neither sufficient corrosion resistance nor workability, and is also inferior in film removability. This is because the amount of tungsten relatively decreases, thus failing to sufficiently form a passive film, while the amount of silicate relatively increases to form a firm network structure.
  • the obtained film can achieve neither sufficient corrosion resistance nor workability. This is because the amount of the water-soluble silicate relatively decreases, thus making it easier to transmit moisture, while crystals of tungsten are precipitated, thus degrading adhesion and uniformity of the coating film.
  • a lubricating coating agent containing a water-soluble silicate and a water-soluble tungstate may be prepared, followed by application to a surface of a steel wire rod.
  • a mass ratio of water-soluble tungstate/water-soluble silicate in the lubricating coating film is the same as that of water-soluble tungstate/water-soluble silicate in the lubricating coating agent.
  • the lubricating coating film may be formed using a composition prepared by mixing a water-soluble silicate and a water-soluble tungstate so as to adjust a mass ratio of water-soluble tungstate/water-soluble silicate in the lubricating coating film in a range of 0.7 to 10.
  • a mass ratio tungsten/silicon is preferably 1.3 or more, more preferably 1.8 or more, and still more preferably 2.0 or more.
  • the mass ratio is preferably 18 or less, more preferably 10 or less, and still more preferably 5.4 or less.
  • the obtained film can achieve neither sufficient corrosion resistance nor workability, and is also inferior in film removability. This is because the amount of the tungstate relatively decreases, thus failing to sufficiently form a passive film, while the amount of the silicate relatively increases to form a firm network structure. If the mass ratio of tungsten/silicon is more than 18, the obtained film can achieve neither sufficient corrosion resistance nor workability. This is because the amount of the silicate relatively decreases, thus making it easier to transmit moisture, while crystals of tungsten are precipitated, thus degrading adhesion and uniformity of the film.
  • the mass ratio of tungsten/silicon is based on a ratio of tungsten element derived from the water-soluble tungstate to a silicon element derived from the water-soluble silicate in the film and can be calculated, for example, using inductively coupled plasma or fluorescent X-ray spectroscopy.
  • water-soluble silicate used in the lubricating coating agent examples include lithium silicate, sodium silicate and potassium silicate. These water-soluble silicates may be used alone, or two or more water-soluble silicates may be used.
  • water-soluble tungstate used in the lubricating coating agent examples include lithium tungstate, sodium tungstate, potassium tungstate, and ammonium tungstate. These water-soluble tungstates may be used alone, or two or more water-soluble tungstates may be used.
  • the resin is mixed in the coating film for the purpose of the binder effect, an improvement in adhesion between a base material and a film, imparting of leveling property by the thickening effect, and stabilization of a dispersion component.
  • the resin having such function and property include a vinyl resin, an acrylic resin, an epoxy resin, a urethane resin, a phenol resin, a cellulose derivative, a polymaleic acid and a polyester resin. These resins may be used alone, or two or more resins may be used in combination.
  • the lubricating coating film contains a resin and a mass ratio of resin/(water-soluble silicate and water-soluble tungstate) is preferably 0.01 or more, and more preferably 0.05 or more.
  • the mass ratio is preferably 1.5 or less, and more preferably 1.0 or less. If the mass ratio is less than 0.01, the above effects are not sufficiently exerted. Meanwhile, if the mass ratio exceeds 1.5, the amounts of the water-soluble silicate and the water-soluble tungstate relatively decrease, thus failing to realize sufficient workability and corrosion resistance.
  • the lubricant itself has slipperiness, and has a function of reducing a friction force. In general, if the friction force increases during plastic working, an increase in working energy, heat generation, seizure, and the like occur. It the lubricant is included in a lubricating coating agent used in the present invention, the lubricant exists in a lubricating coating film in the form of a solid, thus suppressing an increase in friction force.
  • the lubricant having such function and property include wax, polytetrafluoroethylene, fatty acid soap, fatty acid metal soap, fatty acid amide, molybdenum disulfide, tungsten disulfide, graphite and melamine cyanurate. These lubricants may be used alone, or two or more lubricants may be used in combination.
  • the wax include polyethylene wax, paraffin wax, microcrystalline wax, polypropylene wax, and carnauba wax.
  • Specific examples of the fatty acid soap include sodium myristate, potassium myristate, sodium palmitate, potassium palmitate, sodium stearate and potassium stearate.
  • Specific examples of the fatty acid metal soap include calcium stearate, zinc stearate, barium stearate, magnesium stearate, and lithium stearate.
  • the fatty acid amide is, for example, an amide compound having two fatty acids, and specific examples thereof include ethylenebislauric acid amide, ethylenebisstearic acid amide, ethylenebisbehenic acid amide, N,N′-distearyladipic acid amide, ethylenebisoleic acid amide, ethylenebiserucic acid amide, hexamethylenebisoleic acid amide, and N,N′-dioleyladipic acid amide.
  • the mass ratio of lubricant/(water-soluble silicate and water-soluble tungstate) is preferably 0.01 or more, and more preferably 0.05 or more, and the mass ratio is preferably 1.5 or less, and more preferably 1.0 or less.
  • the mass ratio of lubricant/(water-soluble silicate+water-soluble tungstate) is less than 0.01, it is impossible to perform performances because of too small amount of the lubricant. If the mass ratio exceeds 1.5, the amounts of the water-soluble silicate and the water-soluble tungstate relatively decrease, thus failing to exhibit high corrosion resistance and workability which are features of the present invention.
  • the lubricating coating film of the steel wire rod of the present invention can be mixed with a viscosity modifier, in addition to the water-soluble silicate, the water-soluble tungstate, the resin, and the lubricant, for the purpose of imparting leveling property and thixotrophy so as to ensure a uniform coating state when a lubricating treatment solution is applied to a base material.
  • the amount of the viscosity modifier is preferably in a range of 0.1 to 30% by mass based on the mass of total solid component.
  • the viscosity modifier examples include smectite-based clay minerals such as montmorillonite, sauconite, beidellite, hectorite, nontronite, saponite, iron-rich saponite, and stevensite; and inorganic thickeners such as pulverized silica, bentonite, and kaolin.
  • smectite-based clay minerals such as montmorillonite, sauconite, beidellite, hectorite, nontronite, saponite, iron-rich saponite, and stevensite
  • inorganic thickeners such as pulverized silica, bentonite, and kaolin.
  • the lubricating coating film may contain water-soluble salts, for example, inorganic salts, such as sulfates and borates, and organic salts so as to improve adhesion and workability.
  • inorganic salts such as sulfates and borates
  • organic salts so as to improve adhesion and workability.
  • the sulfate include sodium sulfate, potassium sulfate, and the like.
  • the borate include sodium metaborate, potassium metaborate, ammonium metaborate, and the like.
  • organic salt examples include salts of formic acid, acetic acid, butyric acid, oxalic acid, succinic acid, lactic acid, ascorbic acid, tartaric acid, citric acid, malic acid, malonic acid, maleic acid, phthalic acid, and the like, with alkali metals, alkali earth metals, and the like.
  • the lubricating coating film of the steel wire rod of the present invention can be imparted with high corrosion resistance before and after working, and may be mixed with other water-soluble rust preventives and inhibitors for the purpose of further improving corrosion resistance.
  • rust preventives and inhibitors for example, various organic acids such as oleic acid, dimer acid, tartaric acid, and citric acid; various chelating agents such as EDTA, NTA, HEDTA, and DTPA; mixed components of alkanolamine such as triethanolamine, and amine salts of p-t-butylbenzoic acid; and combinations of a carboxylic acid amine salt, a dibasic acid amine salt, an alkenylsuccinic acid, and a water-soluble salt thereof with aminotetrazole and a water-soluble salt thereof.
  • These rust preventives and inhibitors may be used alone, or two or more rust preventives and inhibitors may be used in combination.
  • the amount is preferably in a range of
  • the lubricating coating agent contains the water-soluble silicate and the water-soluble tungstate as essential components, and optionally contains the above-mentioned resin, lubricant, and water-soluble salts.
  • the amount of the water-soluble silicate preferably exceeds 5% by mass, more preferably 10% by mass or more, and still more preferably 15% by mass or more, and is also preferably 58% by mass or less, more preferably 52% by mass or less, and still more preferably 45% by mass or less, in 100% by mass of the lubricating coating agent.
  • the amount of the water-soluble tungstate is preferably 10% by mass or more, more preferably 15% by mass or more, and still more preferably 20% by mass or more, and is also preferably 91% by mass or less, more preferably 85% by mass or less, and still more preferably 80% by mass or less, in 100% by mass of the lubricating coating agent.
  • the obtained film cannot achieve sufficient long-term rust prevention property, and is inferior in wire drawability and ball ironing property. This is because the amount of the water-soluble silicate relatively decreases, thus making it easier to transmit moisture, while crystals of tungsten are precipitated, thus degrading adhesion and uniformity of the coating film. If the amount of the water-soluble silicate exceeds 58% by mass and the amount of the water-soluble tungstate is less than 10% by mass, the obtained film can achieve neither sufficient corrosion resistance nor workability. This is because the amount of tungsten relatively decreases, thus failing to sufficiently form a passive film, while the amount of silicate relatively increases to form a firm network structure.
  • the lubricating coating film may also be formed as a lubricating undercoating film for dry lubricant.
  • a dry lubricant enables leveling up of lubricity, seize resistance, and corrosion resistance.
  • a general lubricating powder or wire drawing powder which contains, as main components, higher fatty acid soap, borax, lime, molybdenum disulfide, and the like.
  • a liquid medium (solvent, dispersion medium) for formation of a lubricating coating film in a film treatment agent is water.
  • the lubricating coating agent may contain a water-soluble strong alkali component.
  • a water-soluble strong alkali component include lithium hydroxide, sodium hydroxide and potassium hydroxide. These water-soluble strong alkali components may be used alone, or two or more water-soluble strong alkali components may be used in combination. The amount of these water-soluble strong alkali components is preferably in a range of 0.01 to 10% by mass based on the mass of total solid component.
  • the lubricating coating agent used in the present invention is produced by adding a water-soluble silicate and a water-soluble tungstate, and a resin and a lubricant, and if necessary a viscosity modifier to water as a liquid medium, followed by mixing.
  • the water-soluble silicate and the water-soluble tungstate used herein are soluble in water, but some of the resin, the lubricant, the viscosity modifier, and the like are insoluble or slightly soluble in water, so that there is a need to disperse them in the lubricating coating agent.
  • a surfactant capable of serving as a dispersant is optionally added to water and, after sufficiently maintaining the surfactant in close association with water, stirring is continued until a dispersed state becomes uniform.
  • Stirring is performed by a general method such as propeller stirring or stirring with a homogenizer.
  • known surfactants can be used.
  • a method for producing a steel wire rod according to the present invention will be described below.
  • the method according to the present invention includes a cleaning step of a steel wire rod, a production step of a film treatment agent, and a drying step. Each step will be described below.
  • At least one cleaning treatment selected from shot blasting, sand blasting, wet blasting, peeling, alkali degreasing, and pickling is preferably performed. Cleaning as used herein is performed for the purpose of removing oxide scales grown by annealing, and various contaminations (oils, etc.).
  • a production step of a lubricating coating film on a steel wire rod there is no particular limitation on a production step of a lubricating coating film on a steel wire rod, and it is possible to use coating methods such as an immersion method, a flow coating method, and a spraying method.
  • Coating is not particularly limited as long as a surface of the steel wire rod is sufficiently coated with a lubricating coating agent of the present invention, and also the coating time is not particularly limited.
  • the steel wire rod may be brought into contact with the lubricating coating agent after heating to a temperature in a range of 60 to 80° C.
  • the steel wire rod may also be brought into contact with the lubricating coating agent heated to a temperature in a range of 40 to 70° C. Whereby, the drying property may be sometimes improved significantly, thus enabling drying at a normal temperature and reduction in thermal energy loss.
  • Drying may be performed by being left to stand at a normal temperature, or may performed at 60 to 150° C. for 1 to 30 minutes.
  • the mass of a lubricating coating film formed on a steel wire rod is appropriately controlled by the degree of subsequent working, and the mass of the coating film is preferably 1.0 g/m 2 or more, more preferably 2.0 g/m 2 or more, and is also preferably 20 g/m 2 or less, and more preferably 15 g/m 2 or less.
  • Low mass of the coating film leads to insufficient workability. It is not preferred that the mass of the coating film exceeds 20 g/m 2 since clogging occurs in a die, although there is no problem in workability.
  • the mass of the coating film can be calculated from a difference in mass between steel wire rods before and after a treatment, and a surface area.
  • the solid component mass (concentration) of the lubricating coating agent is appropriately adjusted.
  • the thus obtained treatment solution is often used.
  • water used for dilution and adjustment and, for example, pure water, deionized water, tap water, ground water, industrial water, and the like can be used.
  • film removal can be performed by immersing the lubricating coating film formed of the lubricating coating agent in an aqueous alkali cleaner, or spraying the aqueous alkali cleaner.
  • the alkali cleaner is a solution prepared by dissolving a common alkali component such as sodium hydroxide or potassium hydroxide in water and, when the alkali cleaner is brought into contact with the lubricating coating film, the lubricating coating film dissolves in the cleaning solution, thus making it possible to easily perform film removal. It is also possible to obtain a film capable of easily falling off by a heat treatment after working. Therefore, alkali cleaning and heat treatment enable prevention of contamination and poor plating in the subsequent step caused by insufficient film removal.
  • lubricating coating agents of Examples 1 to 18 and Comparative Examples 1 to 12 were prepared using the respective components shown in Table 1.
  • Comparative Example 13 means the case subjected to a phosphate/soap treatment.
  • C-1 Polyvinyl alcohol (average molecular weight of about 50,000)
  • C-2 Sodium neutralizing salt of isobutylene-maleic anhydride copolymer (average molecular weight of about 165,000)
  • Example 1 Water-soluble silicate Water-soluble tungstate Resin Lubricant Undercoating Component (A) Component (B) Component (C) Component (D) film (A-1) (A-2) (A-3) (B-1) (B-2) (B-3) (C-1) (C-2) (D-1) (D-2) (F-1)
  • Example 1 40 15 0 45 0 0 0 0 0 0 None Example 2 0 25 0 0 75 0 0 0 0 0 None Example 3 30 20 5 0 0 45 0 0 0 0 None Example 4 9 0 0 25 30 30 6 0 0 0 0 None Example 5 10 0 30 38 0 0 2 0 20 0 None Example 6 0 0 0 20 0 30 20 0 10 10 10 None Example 7 40 0 0 0 50 0 7 0 0 3 None Example 8 0 45 0 0 20 30 0 0 5 0 None Example 9 10 0 5 17 0 10 18
  • Each lubricating coating treatment was carried out by the following steps, with respect to a surface of a ⁇ 3.2 mm sample steel wire rod (steel type: S45C). After subjecting to the lubricating coating treatment, a mass ratio of water-soluble tungstate/water-soluble silicate in a lubricating coating film of a sample steel wire rod is the same as a mass ratio of water-soluble tungstate/water-soluble silicate in a lubricating coating agent mentioned in Table 1.
  • the amount of a lubricating coating film was appropriately adjusted by the concentration of a treatment agent.
  • Wire drawing was performed by drawing a sample wire rod in size of ⁇ 3.2 mm ⁇ 20 m through a ⁇ 2.76 die. Missile C40 available from Matsuura Kougyo K.K. was used as a dry lubricant. Immediately before drawing a material, a die box was charged with the dry lubricant so that the dry lubricant naturally adheres to the material. Evaluation was made from seizure of the test material and the remaining amount of the lubricating coating film after wire drawing. In wire drawing of the phosphate/soap coating film of Comparative Example 13, the dry lubricant is not used in accordance with a normal usage manner.
  • A No seizure occurs and no metal gloss is recognized and, on the whole, a film remains in a large amount.
  • B No seizure occurs and no metal gloss is recognized, and a film remains in an amount which slightly smaller than that in A.
  • C No seizure occurs and a film retention amount is slightly small, and metal gloss is partially recognized.
  • D No seizure occurs and metal gloss is recognized at numerous sites.
  • E Seizure occurred.
  • Comparative Examples 2 to 9 in which a ratio of a water-soluble silicate to a water-soluble tungstate deviates from the scope of the present invention, workability was inferior and also corrosion resistance was inferior because of small film retention amount after wire drawing.
  • Comparative Examples 10 to 12 in which components other than the silicate and tungstate were included as aqueous inorganic salts, workability was inferior and also corrosion resistance was inferior because of small film retention amount after wire drawing.
  • Comparative Example 13 in which the phosphate coating film was subjected to a reactive soap treatment comparatively excellent performances were exhibited.
  • Comparative Example 13 deviates from the object of the present invention.
  • Comparative Examples 9 and 10 deviate from the scope of the present invention because of containing phosphorus.
  • lubricating coating agents of Examples 19 to 38 and Comparative Examples 14 to 25 were prepared using the respective components shown below.
  • Comparative Example 26 means the case subjected to a phosphate/soap treatment.
  • C-1 Polyvinyl alcohol (average molecular weight of about 50,000)
  • C-2) Sodium neutralizing salt of isobutylene-maleic anhydride copolymer (average molecular weight of about 165,000)
  • C-3) Carboxymethylcellullose sodium (average molecular weight of about 30,000)
  • C-4) Aqueous nonionic urethane resin emulsion
  • D-1 Anionic polyethylene wax (average particle size of 5 ⁇ m)
  • D-2) Ethylenebis-stearic acid amide
  • D-3) Calcium stearate
  • D-4) Polytetrafluoroethylene dispersion (average particle size of 0.2 ⁇ m)
  • a mass ratio of water-soluble tungstate/water-soluble silicate in a lubricating coating film of a sample steel wire rod is the same as a mass ratio of water-soluble tungstate/water-soluble silicate in a lubricating coating agent mentioned in Table 3.
  • the amount of a lubricating coating film was appropriately adjusted by the concentration of a treatment agent.
  • a spike test was performed as a test on the hypothesis of shank reducing when a steel wire is formed into a bolt.
  • the spike test was performed in accordance with the method defined in JP 05-7969 A. After the test, lubricity was evaluated by a spike height and a forming load. The more the spike height increases and the more the forming load decreases, the more lubricity becomes excellent. As mentioned in the above document, an area expansion ratio in the spike test is about 10 times. Lubricity of the film was evaluated by measuring the load and the spike height during working.
  • Test piece for evaluation S45C spheroidizing-annealed material in size of 25 mm ⁇ 30 mm
  • Spike performance spike height (mm)/working load (kNf) ⁇ 100
  • An upsetting-ball ironing test was performed as a test on the hypothesis of forming of a bolt head when a steel wire is formed into a flange bolt.
  • the upsetting-ball ironing test was performed in accordance with the method defined in JP 2013-215773 A.
  • An area expansion ratio in the upsetting-ball ironing test was adjusted to at most 150 or more times, and the area expansion ratio is very large as compared with the above-mentioned spike test. Therefore, it is a test capable of reproducing working that requires high workability for formation of a head part of a hexagon bolt with flange.
  • Seizure resistance of the coating film was evaluated by evaluating the amount of seizure of an ironing surface.
  • Test piece for evaluation S10C spheroidizing-annealed material in size of 14 mm ⁇ 32 mm
  • a film removability test was performed as follows. Using an upper mold and a lower mold, each having a plane surface, a columnar test piece was subjected to upsetting at a compression ratio of 50%, and then immersed in an alkali cleaner mentioned below. A film retention ratio was calculated by measuring the weight of a coating film before and after a film removal treatment.
  • Test piece for evaluation S45C spheroidizing-annealed material in size of 25 mm ⁇ 30 mm
  • Alkali cleaner aqueous 2% NaOH solution
  • Film removal conditions liquid temperature: 60° C., immersion: time: 2 minutes
  • Film retention ratio (%) (film weight after film removal treatment/film weight before film removal treatment) ⁇ 100
  • a film retention ratio is 0%
  • B A film retention ratio exceeds 0% and less than 8%
  • C A film retention ratio 8% or more and less than 16%
  • D A film retention ratio is 16% or more and less than 25%
  • E A film retention ratio is 25% or more
  • Test piece SPCC-SD in size of 75 mm ⁇ 35 mm ⁇ 0.8 mm Evaluation criteria: A: Extremely excellent as compared with a phosphate/soap coating film (rust area of 3% or less) B: Excellent as compared with a phosphate/soap coating film (rust area of exceeding 3% to 10% or less) C: Identical to a phosphate/soap coating film (rust area of exceeding 10% to 20% or less) D: Inferior to a phosphate/soap coating film (rust area of exceeding 20% to 30% or less) E: Drastically inferior as compared with a phosphate/soap coating film (rust area of exceeding 30%)
  • Comparative Example 26 in which the phosphate coating film was subjected to a reactive soap treatment, comparatively excellent performances were exhibited.
  • Comparative Example 26 because of containing phosphorus, when subjecting to a heat treatment such as quenching and tempering while having the lubricating coating film on a surface, there is a fear that the steel wire rod becomes fragile as a result of the occurrence of phosphorizing. Therefore, Comparative Example 26 deviates from the object of the present invention.
  • Comparative Examples 19 and 22 deviate from the scope of the present invention because of containing phosphorus.
  • the lubricating coating film contains a water-soluble silicate but contains no water-soluble tungstate, insufficient film removability was exhibited.
  • the steel wire rod of the present invention does not exhibit phosphorizing property during a heat treatment because of containing no phosphorus, and also can reconcile high workability and corrosion resistance which are equal to or better than those of the steel wire rod subjected to conventional phosphate and soap treatments. Because of satisfactory film removability of the lubricating coating film due to a cleaner after working, the steel wire rod of the present invention also contributes to an improvement in process efficiency when the subsequent step such as a plating step is performed after forming into a bolt. Therefore, the steel wire rod of the present invention has an industrially high utilization value.
  • the present invention includes the following aspects.
  • a steel wire rod including a lubricating coating film on a surface, wherein the lubricating coating film contains a water-soluble silicate and a water-soluble tungstate, a mass ratio of water-soluble tungstate/water-soluble silicate being in a range of 0.7 to 10, and contains no phosphorus.
  • a steel wire rod including a lubricating coating film containing no phosphorus, wherein
  • the lubricating coating film is formed using a composition prepared by mixing a water-soluble silicate and a water-soluble tungstate so as to adjust a mass ratio of water-soluble tungstate/water-soluble silicate in the lubricating coating film in a range of 0.7 to 10.
  • the steel wire rod according to aspect 1 or 2 wherein the lubricating coating film contains a resin, and a mass ratio of resin/(water-soluble silicate+water-soluble tungstate) is in a range of 0.01 to 1.5.

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  • Oil, Petroleum & Natural Gas (AREA)
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  • Chemical Treatment Of Metals (AREA)
US15/129,321 2014-03-28 2015-03-20 Steel wire rod having lubricating coating film that has excellent corrosion resistance and workability Abandoned US20170175021A1 (en)

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JP2014-070446 2014-03-28
JP2014070446A JP2015189952A (ja) 2014-03-28 2014-03-28 耐食性及び加工性に優れた潤滑皮膜を有する鋼線材
PCT/JP2015/058556 WO2015146848A1 (ja) 2014-03-28 2015-03-20 耐食性及び加工性に優れた潤滑皮膜を有する鋼線材

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US20180273869A1 (en) * 2015-09-30 2018-09-27 Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd.) Steel wire with excellent corrosion resistance and appearance after processing
US20190003000A1 (en) * 2015-06-29 2019-01-03 Nippon Steel & Sumitomo Metal Corporation Bolt
EP3434808A4 (en) * 2016-03-22 2019-03-20 Sumitomo (SEI) Steel Wire Corp. OIL FILM WIRE

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JP7142498B2 (ja) * 2018-06-28 2022-09-27 日本パーカライジング株式会社 金属材料用表面処理剤並びに、表面処理被膜付金属材料及びその製造方法
JP6933294B2 (ja) * 2018-08-07 2021-09-08 Ｊｆｅスチール株式会社 潤滑皮膜を有する鋼板およびその製造方法
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KR102132479B1 (ko) * 2019-06-26 2020-08-06 세븐그램(주) 선재 윤활 코팅제 및 그 제조 방법
JP6839315B1 (ja) * 2020-03-17 2021-03-03 有限会社中川商会 被処理物の表面改質方法
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CN114908303B (zh) * 2022-04-28 2022-11-15 宁波金鼎紧固件有限公司 一种紧固件用复合材料及其制备方法

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JPH08151592A (ja) * 1994-11-30 1996-06-11 Mitsubishi Heavy Ind Ltd 潤滑皮膜材、潤滑皮膜の製造方法及び潤滑皮膜を施したボルト・ナット
JP4031213B2 (ja) * 2001-06-07 2008-01-09 株式会社神戸製鋼所 皮膜形成剤及び皮膜
JP2006161126A (ja) * 2004-12-09 2006-06-22 Sumitomo Metal Ind Ltd 化成処理性に優れた潤滑処理鋼板
JP4386450B2 (ja) * 2005-03-03 2009-12-16 株式会社神戸製鋼所 塑性加工用金属材料およびその製造方法ならびに塑性加工用金属材料の表面処理剤
JP5682021B2 (ja) * 2010-05-25 2015-03-11 日本パーカライジング株式会社 難結晶性を有し、耐吸湿性、耐食性及び加工性に優れる金属材料塑性加工用水系潤滑剤及びその潤滑皮膜を形成させた金属材料

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US20190003000A1 (en) * 2015-06-29 2019-01-03 Nippon Steel & Sumitomo Metal Corporation Bolt
US10669604B2 (en) * 2015-06-29 2020-06-02 Nippon Steel Corporation Bolt
US20180273869A1 (en) * 2015-09-30 2018-09-27 Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd.) Steel wire with excellent corrosion resistance and appearance after processing
EP3434808A4 (en) * 2016-03-22 2019-03-20 Sumitomo (SEI) Steel Wire Corp. OIL FILM WIRE
US10760028B2 (en) 2016-03-22 2020-09-01 Sumitomo Electric Industries, Ltd. Oil tempered wires

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KR101817456B1 (ko) 2018-01-10
KR20160125504A (ko) 2016-10-31

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