EP0412788A1 - Méthode de lubrification pour traitement de matériaux mÀ©talliques lors du travail plastique à froid - Google Patents

Méthode de lubrification pour traitement de matériaux mÀ©talliques lors du travail plastique à froid Download PDF

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Publication number
EP0412788A1
EP0412788A1 EP90308707A EP90308707A EP0412788A1 EP 0412788 A1 EP0412788 A1 EP 0412788A1 EP 90308707 A EP90308707 A EP 90308707A EP 90308707 A EP90308707 A EP 90308707A EP 0412788 A1 EP0412788 A1 EP 0412788A1
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EP
European Patent Office
Prior art keywords
treatment liquid
aqueous
lubrication treatment
metallic
aqueous lubrication
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.)
Granted
Application number
EP90308707A
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German (de)
English (en)
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EP0412788B1 (fr
Inventor
Hiroyuki C/O Nippondenso Co. Ltd. Fujii
Takanori C/O Nippondenso Co. Ltd. Mizutani
Tokuo C/O Nippondenso Co. Ltd. Shirai
Yoshio C/O Nihon Parkerizing Company Ltd. Nagae
Kouji C/O Nihon Parkerizing Company Ltd Kaburaki
Kouji C/O Nihon Parkerizing Company Ltd Hetsugi
Yasuo C/O Nihon Parkerizing Company Ltd Tanizawa
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Nihon Parkerizing Co Ltd
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Nihon Parkerizing Co Ltd
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    • C10M173/00—Lubricating compositions containing more than 10% water
    • C10M173/02—Lubricating compositions containing more than 10% water not containing mineral or fatty oils
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    • C10M129/26—Carboxylic acids; Salts thereof
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    • C10M129/38—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms
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    • 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
    • C10N2040/241—Manufacturing joint-less pipes
    • 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
    • C10N2040/242—Hot working
    • 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
    • C10N2040/243—Cold working
    • 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
    • C10N2040/244—Metal working of specific metals
    • 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
    • C10N2040/244—Metal working of specific metals
    • C10N2040/245—Soft metals, e.g. aluminum
    • 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
    • C10N2040/244—Metal working of specific metals
    • C10N2040/246—Iron or steel
    • 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
    • C10N2040/244—Metal working of specific metals
    • C10N2040/247—Stainless steel
    • 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
    • C10N2050/01—Emulsions, colloids, or micelles

Definitions

  • This invention relates to an aqueous lubrica­tion treatment liquid for cold plastic working metallic materials.
  • this invention relates to an aqueous lubrication treatment liquid for a cold plastic working (forging, tube drawing, wire drawing, etc.) of metallic materials, for example, steel, stainless steels, titanium-based alloys, copper, copper-based alloys, aluminum, aluminum-based alloys, etc. (hereinafter referred to as an aqueous lubrication treatment liquid).
  • a cold plastic working forging, tube drawing, wire drawing, etc.
  • metallic materials for example, steel, stainless steels, titanium-based alloys, copper, copper-based alloys, aluminum, aluminum-based alloys, etc.
  • liquids which comprise a solid lubricant for example, molybdenum disulfide or graphite, at least one member selected from inorganic binders and organic binders, and a surfactant are known.
  • a method is employed of forming a solid lubricant film over a chemical conversion coating where a metallic material surface, after the formation of the chemical conversion coating, is brought into contact with an aqueous lubrication treatment liquid, followed by drying, or has a solid lubricant powder deposited thereon.
  • a solid lubricant in a powder state causes a problem of a deterioration of the working environment, and thus most preferably a lubricant in the form of an aqueous treatment liquid is used.
  • a conventional aqueous lubricant treatment liquid has a drawback in that it has an unstable and insufficient lubricating property and causes rusting of the treated or formed metallic material when left to stand after the lubricating treatment or a plastic working.
  • An object of the present invention is to provide an aqueous lubrication treatment liquid for cold plastic working metallic materials, which liquid does not have the above-mentioned disadvantages of conventional aqueous lubrication treatment liquids and exhibits a high stability and an excellent lubricating property, without causing a rusting of the metallic materials.
  • the aqueous lubrication treatment liquid of the present invention for cold plastic working metallic materials which comprises 4 to 160 g/l of a metallic soap, 50 to 400 g/l of a solid lubricant, 0.5 to 40 g/l of a surfactant for uniformly dispersing the metallic soap and the solid lubricant, and water.
  • the aqueous lubrication treatment liquid of the present invention optionally further comprises a colloidal titanium compound in an amount of 10 ppm or more, in the terms of titanium.
  • the aqueous lubrication treatment liquid of the present invention optionally further comprises 5 to 150 g/l of a binder.
  • the inventors of the present invention found for the first time that a lubricating film having an excellent lubricating activity not obtained by the conventional aqueous lubrication treatment liquid can be formed on a surface of a metallic article by applying a new type of aqueous lubrication treatment liquid comprising a metallic soap, a solid lubricant, and a surfactant.
  • aqueous lubrica­tion treatment liquid containing a colloidal titanium compound in addition to the above-mentioned component is useful for forming a lubricating film having an excellent lubricating property and a superior resistance to rust on a surface of metallic article, for example, a cold plastic processed steel article.
  • an addition of a binder to the metallic soap, solid lubricant, surfactant, and optionally, colloidal titanium compound is effective for further enhancing the lubricating property thereof, due to the synergistic effect of the binder with the other components, for example, the metallic soap and the colloidal titanium compound.
  • the present invention was completed based on the above-mentioned findings.
  • the aqueous lubrication treatment liquid of the present invention comprises, as principal components, 4 to 160 g/l of a metallic soap, 50 to 400 g/l of a solid lubricant, 0.5 to 40 g/l of a surfactant for uniformly dispersing the metallic soap and the solid lubricant in water, and water.
  • the metallic soap usable for the present invention comprises at least one member selected from salts of fatty acids and hydroxy-fatty acids having 12 to 22 carbon atoms with multivalent metals.
  • the fatty acids and the hydroxy-fatty acids usable for the present invention include lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, and hydroxystearic acids.
  • a preferable fatty acid is stearic acid.
  • the multivalent metals usable for the present invention are selected from calcium, aluminum, magnesium, barium, and zinc.
  • a preferable metallic soap for the present inven­tion is a wet state calcium stearate prepared in accordance with Japanese Examined Patent Publication No. 60-45680.
  • the metallic soap is contained in a dry content of 4 to 160 g/l, preferably 10 to 50 g/l in the aqueous lubrication treatment liquid. If the metallic soap is employed in an amount of less than 4 g/l, the resultant lubricating film on a metallic article exhibits an unsatisfactory lubricating effect. Also, even if the content of the metallic soap is increased to a level above 160 g/l, the lubricating effect of the resultant lubricating film on a metallic article is substantially not increased higher than that resulted from 160 g/l of the metallic soap; rather the lubricating effect of the solid lubricant is restricted by the large amount of the metallic soap.
  • the solid lubricant usable for the present invention comprises at least one member selected from, for example, molybdenum disulfide, graphite, tungsten disulfide, fluorinated graphite, boron nitride, and talc.
  • the content of solid lubricant in the treatment liquid is 50 to 400 g/l, preferably 150 to 250 g/l.
  • a content of the solid lubricant of less than 50 g/l does not provide a sufficient formation of a solid lubricating film on the metallic article surface. If the content of the solid lubricant is more than 400 g/l, the lubrication effect becomes saturated so that no further improvement of the lubrication effect is obtained, and the cost of the aqueous lubrication liquid is increased.
  • the aqueous lubrication treatment liquid of the present invention when the metallic soap is employed in a mixing weight ratio of from 2:5 to 1:50 to the solid lubricant, the resultant lubricating film on the metallic article exhibits an excellent lubricating effect.
  • a surfactant is employed for dis­persing the metallic soap and solid lubricant in water.
  • a surfactant is employed for dis­persing the metallic soap and solid lubricant in water.
  • Surfactants in general use include nonionic type surfactants, for example, polyoxyethylene alkyl ethers, polyoxyethylene alkylphenyl ethers, polyoxyethylene alkyl esters, and polyoxyethylene sorbitane alkyl esters; anionic type surfactants, for example, fatty acid salts, alkyl sulphates, alkyl sulphonate, alkyl phosphates and alkyl dithiophosphates; cationic type surfactants, for example, aliphatic amine salts, and quarternary ammonium salts; and amphoteric type surfactants, for example, amino acid type and betain type carboxylic acid salts, sulfuric ester salts, sulphonic ester salts, and phosphoric ester salts.
  • anionic type surfactants for example, fatty acid salts, alkyl sulphates, alkyl sulphonate, alkyl phosphates and alkyl dithiophosphates
  • the content of the surfactant in the aqueous lubrication liquid of the present invention is 0.5 to 40 g/l, preferably 5 to 10 g/l.
  • the content of the surfactant in the aqueous lubrication treatment liquid is preferably increased or decreased in response to the content of the solid lubricant. Where the content of surfactant is less than 0.5 g/l, the solid surfactant in the treatment liquid is insufficiently wetted, and a greater quantity than 40 g/l does not increase the dispersing effect of the surfactant to any significant degree.
  • the aqueous lubrication treatment liquid of the present invention can be supplemented with another additive, for example, a high molecular dispersing agent, defoaming agent, and rust-preventive additive.
  • another additive for example, a high molecular dispersing agent, defoaming agent, and rust-preventive additive.
  • the aqueous lubrication treatment liquid of the present invention optionally contains a colloidal titanium compound in addition to the above-mentioned components.
  • the colloidal titanium compound is preferably in a state of a cloudy solution prepared, for example, by neutralizing a compound of sulphuric acid with titanium or of phosphoric acid with titanium, with an alkali, for example, caustic soda or the like.
  • the content of colloidal titanium in the aqueous lubrication treatment liquid is 10 ppm or more, preferably 10 to 5000 ppm, more preferably 50 to 300 ppm, in terms of titanium.
  • the content of colloidal titanium compound in the aqueous lubrication liquid of this invention has no specific upper limit: it is possible to increase the content to a high level as long as the preparation of the aqueous lubrication treatment liquid is possible. Nevertheless, the colloidal titanium compound is usually employed in a content of from 10 to 5000 ppm.
  • the colloidal titanium compound usable for the present invention is in the form of colloidal particles consisting of negatively charged micelles. Accordingly, the colloidal titanium compound is definitely distinct from fine particles of titanium compounds, for example, titanium dioxide, usable for pigments, which particles are produced by finely pulberizing grains of the compounds, and the resultant particles do not have an electrical charge when dispersed in water.
  • the aqueous lubrication treatment liquid optionally contains a binder in addition to the above-mentioned components.
  • the binder comprises at least one member selected from inorganic and organic binder materials and is effective for further enhancing the lubricating effect of the resultant lubricating film on the metallic article surface.
  • the inorganic binder is not restricted to a specific type of binder and preferably comprises at least one member selected from the borates, phosphates, and silicates mentioned below.
  • the organic binder is not limited to a specific type of binder, and preferably comprises at least one member selected from water-soluble high molecular compounds, for example, natural high molecular substance much as starch, sea weeds, vegetable mucilages, animal proteins, and fermentation mucilages; semi-synthetic high molecular substances prepared from starch and cellulose; and synthetic polymers, for example, polyvinyl pyrrolidone, polyethylene glycol, and polyvinyl alcohol.
  • water-soluble high molecular compounds for example, natural high molecular substance much as starch, sea weeds, vegetable mucilages, animal proteins, and fermentation mucilages
  • semi-synthetic high molecular substances prepared from starch and cellulose semi-synthetic high molecular substances prepared from starch and cellulose
  • synthetic polymers for example, polyvinyl pyrrolidone, polyethylene glycol, and polyvinyl alcohol.
  • the binder is employed in a solid content of 5 to 150 g/l, preferably 10 to 50 g/l, in the aqueous lubri­cation treatment liquid of the present invention.
  • This solid content is variable depending on the content of the solid lubricant. If the content of the binder is less than 5 g/l, the improvement in the bonding property of the resultant lubricating film to the metallic article surface is not satisfactory. Also, if the binder is employed in a too large content of more than 150 g/l, the resultant aqueous lubrication treatment liquid exhibits an undesirable high viscosity, and thus the amount of the aqueous lubrication treatment liquid adhered to the surface of the metallic article becomes too large. This large amount of the resultant lubri­cating film formed on the metallic article surface causes the metallic die, through/which the metallic article is cold plastic worked, to be clogged.
  • the aqueous lubrication treatment liquid of the present invention can be prepared by dispersing and dissolving the above-mentioned components in predeter­mined amounts in water in the same way as usually practiced.
  • the resultant prepared liquid can be directly used as an aqueous lubrication treatment liquid. If the total content of the components is relatively high, the resultant prepared liquid is directly used or diluted with an additional amount of water and then used as an aqueous lubrication treatment liquid, in response to the type of metallic article, the type of cold plastic working, and the intensity of the working.
  • the metallic article to be treated by the aqueous lubrication treatment liquid is optionally subjected to a chemical conversion procedure before the lubrication treatment.
  • the type of the chemical conversion layer on the metallic material there is no specific restriction of the type of the chemical conversion layer on the metallic material, and, for example, zinc phosphate treatment, iron oxalate treatment, cuprous oxide treatment, aluminum fluoride treatment, and titanium fluoride treatment commonly used according to the type of metals, can be used.
  • the aqueous lubrication treatment liquid of the present invention is applied to a metallic material, usually by an immersion procedure wherein the tempera­ture thereof is maintained at a level between room temperature and 80°C.
  • the metallic article When the aqueous lubrication treatment liquid is applied at a high temperature, the metallic article is also heated, and thus the layer of the aqueous lubrica­tion treatment liquid formed on the metallic article surface can be dried at an enhanced drying efficiency. Nevertheless, if the temperature of the aqueous lubrica­tion treatment liquid becomes too high, the viscosity and concentration of the aqueous lubrication treatment liquid is altered, and thus a complicated control becomes necessary to maintain the viscosity and concen­tration of the aqueous lubrication treatment liquid at a predetermined level by supplying water thereto.
  • the lubrication process using the aqueous lubrica­tion treatment liquid of the present invention usually is carried out in the following sequence.
  • the sequence is variable depending on the type of metallic article, surface condition, type of cold plastic working, and grade of reduction.
  • the degreasing is optionally carried out when necessary.
  • the pickling is carried out to remove rust and scale from the metallic article surface.
  • the metallic article is optionally surface-treated by a shot blast treatment or a sand blast treatment or by the above-mentioned chemical conversion procedure, before the lubrication treatment.
  • the type of surface treatment can be chosen in consideration of the type and surface condition of the metallic article, and the type and intensity of the cold plastic working procedure.
  • the resultant solid lubricating film formed on the metallic article surface or on the chemical conversion layer exhibits an excellent lubricating effect and rust-preventive effect in comparison with that derived from the conventional aqueous lubrication treatment liquid.
  • the present invention offers an aqueous lubrication treatment liquid for cold plastic working of metallic articles by which the metallic articles can be given an excellent lubricating property that enables a satisfac­tory high reduction of a cold plastic working without seizure and galling, with a high workability, and giving the thus processed products a high rust resistance.
  • the carbon steel bar was treated in a solution containing 20 g/l of Fine Cleaner 4360 (trademark of degreasing agent, a product of Nihon Parkerizing Co.) at 70°C for 10 min.
  • Fine Cleaner 4360 trademark of degreasing agent, a product of Nihon Parkerizing Co.
  • the carbon steel bar was treated with running city water at room temperature for 60 sec.
  • the pickling procedure was carried out by using an Ivit 700 A (trademark: made by Asahi Kagaku K.K.) in an amount of 0.05 g/l at room temperature for 10 minutes.
  • the chemical conversion procedure was carried out by immersing the carbon steel bar in an aqueous solution containing a zinc phosphate type chemical conversion film-forming agent (trademark: PB181X, made by Nihon Parkerizing K.K.) in an amount of 90 g/l.
  • a zinc phosphate type chemical conversion film-forming agent (trademark: PB181X, made by Nihon Parkerizing K.K.)
  • An accele­rator for the chemical conversion film-forming agent (trademark: AC131, made by Nihon Parkerizing K.K.) was applied in an amount of 0.3 g/l at a temperature of 80°C for 15 minute, except for Examples 7, 8, 20, and 21 and Comparative Examples 1 and 7, wherein the chemical conversion was not applied.
  • the lubrication treatment was carried out by immersing the carbon steel bar in the aqueous lubrica­tion treatment liquid having the composition as shown in Table 1 at a temperature of 80°C for 3 minutes, except for Comparative Examples 6 and 11, and the treatment was carried out at a temperature of 70°C for 3 minutes.
  • the drying procedure was carried out by blowing hot air at a temperature of 120°C for 10 minutes.
  • the dying procedure can be carried out by leaving the treated metallic article to stand in the ambient atmosphere.
  • the resultant lubrication treated carbon steel bar was subjected to the cold forging test (cold backward cup extrusion test) as indicated in Table 2.
  • the lubricating effect was evaluated by measuring a largest depth of a good inner surface of the extruded cup which could be formed without generating galling or fouling in the form of vertical lines on the inside wall surface of the extruded cup. The greater the deepest depth of the good inner surface of the cup, the better the lubricating effect of the resultant lubricating film on the bar surface.
  • the lubrication treated carbon steel bar was subjected to the rust-resistance test as indicated in Table 3.
  • the rust-resistance was evaluated in the following four classes. Class Evaluation 4 No rust generated. 3 Rust generated in total area corresponding to less than 20% of entire area of surface of specimen. 2 Rust generated in total area corresponding to 20% to 50% of entire area of surface of specimen. 2 Rust generated in total area corresponding to more than 50% of entire area of surface of specimen.
  • Table 1 Cold Backward Cup Extrusion Test Testing machine Cold forging press machine MSF200 (trademark) made by Fukui Kikai K.K. Test condition Test piece S20C ⁇ SUS410L 30 mm ⁇ x 18 - 43 mm (cylinder) Temperature Room temperature Working speed 30 spm Reduction of area 50% Tool Punch 20.2 ⁇ SKH53 Die 30.0 ⁇ SKD11 Table 3 Rust-Resistance Test Testing condition Constant temperature of 50°C constant humidity of 95% Time: 24 hours Testing machine Program constant temperature constant humidity vessel GLMP-62 (Trademark) made by K.K. Futaba Kagaku Specimen Length: 50 mm Diameter: 30 mm
  • the resultant cup depth of the good inner surface was in the range of 30 to 48 mm and greater than that of Comparative Examples 1 to 5, in which the content of the metallic soap was at a low level of 4 g/l or less and in Comparative Examples 2 and 6 in which the content of the solid lubricant was less than 50 g/l. Accordingly, it is clear that the aqueous lubricant treatment liquids of the present invention free from the colloidal titanium compound provide an excellent lubricating effect on the metallic article, which effect was not obtained by the conven­tional aqueous lubrication treatment liquids.
  • Example 7 and 8 in which no chemical conver­sion layer was formed on the carbon steel rod before the lubrication treatment, the resultant cup depth of the good inner surface was 30 to 34 mm, which was a little lower than that in Examples 2 to 6 in which the chemical conversion treatment was applied, and was similar to or a little higher than that in Comparative Example 6, in which a conventional aqueous lubrication treatment liquid was used.
  • the metallic article to be treated was a 13Cr stainless steel bar (SUS 410L, JIS G4303) having a diameter of 30 mm.
  • the pickling was carried out by using an aqueous solution of 7% of HNO3 and 3% of HF at room temperature for 10 minutes.
  • the chemical conversion treatment was carried out by immersing the stainless steel bar in an aqueous solution containing 40 g/l of an oxalate type chemical conversion film-forming agent (trademark: FBA1, made by Nihon Parkerizing K.K.), 20 g/l of an oxalate type chemical conversion film-forming additive (trademark: FBA2, made by Nihon Parkerizing K.K.), and 1 g/l of an oxalate type chemical conversion film-forming accele­rator (trademark: AC-16, made by Nihon Parkerizing K.K.) at a temperature of 90°C for 15 minutes.
  • an oxalate type chemical conversion film-forming agent trademark: FBA1, made by Nihon Parkerizing K.K.
  • FBA2 an oxalate type chemical conversion film-forming additive
  • AC-16 1 g/l of an oxalate type chemical conversion film-forming accele­rator
  • the lubrication treatment was carried out by immersing the stainless steel bar in an aqueous lubrica­tion treatment liquid having the composition as shown in Table 4, at a temperature of 80°C for 3 minutes, except that in Comparative Examples 14 and 18 the immersion treatment was carried out at a temperature of 70°C for 3 minutes.
  • the treated stainless steel bar was subjected to the cold forging test as indicated in Table 2.
  • the depth of the good inner surface of cup was 38 to 54 mm, which is larger than the 28 to 32 mm in Compara­tive Examples 12 to 14. Accordingly, it is clear that, when applied to a stainless steel article, the aqueous lubrication treatment liquid of the present invention exhibits an excellent lubricating effect not obtained by the conventional lubrication treatment liquid.
  • the metallic article to be treated was a titanium wire (Second type, JIS H4600) having a diameter of 3 mm.
  • the pickling was carried out by using an aqueous solution containing 7% of HNO3 and 3% of HF at room temperature for 10 minutes.
  • the chemical conversion treatment was carried out by immersing the titanium wire in an aqueous solution containing 36 g/l of a fluoride type chemical conversion film-forming agent (trademark: MET-3851, made by Nihon Parkerizing K.K.) at a temperature of 60°C for 3 minutes.
  • a fluoride type chemical conversion film-forming agent trademark: MET-3851, made by Nihon Parkerizing K.K.
  • the lubrication treatment was carried out by immersing the titanium wire in an aqueous lubrication treatment liquid having the composition as indicated in Table 5 at a temperature of 80°C for 3 minutes, except that, in Comparative Example 22, the treatment tempera­ture was 70°C.
  • the resultant treated titanium wire was subjected to the cold wire drawing test as indicated in Table 6.
  • Table 6 Wire Drawing Test Testing machine Single head type wire drawing machine Test condition
  • Test piece Titanium (second type) 3 mm ⁇ x 12 mm Temperature Room temperature Drawing speed 50 mm/min Pass condition 1-pass Die diameter 2.7 mm ⁇ , Reduction 19.0% 2-pass Die diameter 2.4 mm ⁇ , Reduction 21.0% 3-pass Die diameter 1.15 mm ⁇ , Reduction 19.7% 4-pass Die diameter 1.9 mm ⁇ , Reduction 21.7% 5-pass Die diameter 1.7 mm ⁇ , Reduction 19.9%
  • Table 5 clearly indicates that, in Examples 29 to 32 in accordance with the present invention, the resul­tant lubrication treated titanium wires exhibited a high resistance to galling even after five passes of the cold drawing test whereas, in Comparative Examples 19 to 22, the resultant lubrication treated titanium wire had galls at the fifth pass of the cold drawing test.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Lubricants (AREA)
  • Metal Extraction Processes (AREA)
  • Mounting, Exchange, And Manufacturing Of Dies (AREA)
EP90308707A 1989-08-09 1990-08-08 Méthode de lubrification pour traitement de matériaux métalliques lors du travail plastique à froid Expired - Lifetime EP0412788B1 (fr)

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JP1204585A JPH0747756B2 (ja) 1989-08-09 1989-08-09 金属の冷間塑性加工用水系潤滑処理液
JP204585/89 1989-08-09

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EP1093510A1 (fr) * 1998-06-09 2001-04-25 Henkel Corporation Composition et procede pour l'enrobage de metaux avec un plastique lubrifie
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WO2001098557A1 (fr) * 2000-06-21 2001-12-27 Henkel Kommanditgesellschaft Auf Aktien Agent adhesif dans des solutions pour conversion
WO2002020704A1 (fr) * 2000-09-05 2002-03-14 Honda Motor Co., Ltd. Agent lubrifiant aqueux de type a un stade pour forgeage a froid efficace
US6455476B1 (en) 1998-06-09 2002-09-24 Henkel Corporation Composition and process for lubricated plastic working of metals
US8541350B2 (en) 2007-11-16 2013-09-24 Henkel Ag & Co. Kgaa Dry-film, anti-corrosive cold forming lubricant
CN105014305A (zh) * 2014-04-21 2015-11-04 哈尔滨飞机工业集团有限责任公司 一种弯边的圆环形薄板的成形方法
US9192973B1 (en) 2013-03-13 2015-11-24 Meier Tool & Engineering, Inc. Drawing process for titanium
CN108602670A (zh) * 2016-01-05 2018-09-28 纳米技术工业解决方案公司 水基纳米颗粒分散体
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CN115612546A (zh) * 2020-06-03 2023-01-17 上海铂斯海特材料科技有限公司 一种水性金属冷挤压润滑剂及其制备工艺

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FR2102283A1 (fr) * 1970-08-15 1972-04-07 Parker Ste Continentale
EP0261438A2 (fr) * 1986-09-23 1988-03-30 Lonza Ag Lubrifiant pour formage d'acier
EP0270836A1 (fr) * 1986-11-10 1988-06-15 Nihon Parkerizing Co., Ltd. Procédé d'étirage de fils
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US6265357B1 (en) 1993-06-24 2001-07-24 Hughes Electronics Corporation High precision, high surface finish broaching method, tool, and lubricant/coolant
WO1995000274A3 (fr) * 1993-06-24 1995-04-20 Hughes Aircraft Co Procede de brochage de precision a finition de surface poussee, outil et agent de lubrification et de refroidissement
US5503506A (en) * 1993-06-24 1996-04-02 Hughes Aircraft Company High precision, high surface finish broaching tool
WO1995000274A2 (fr) * 1993-06-24 1995-01-05 Hughes Aircraft Company Procede de brochage de precision a finition de surface poussee, outil et agent de lubrification et de refroidissement
US5839311A (en) * 1996-09-17 1998-11-24 Minnesota Mining And Manufacturing Company Composition to aid in the forming of metal
US6043201A (en) * 1996-09-17 2000-03-28 Minnesota Mining And Manufacturing Company Composition for cutting and abrasive working of metal
US6294508B1 (en) 1996-09-17 2001-09-25 3M Innovative Properties Company Composition comprising lubricious additive for cutting or abrasive working and a method therefor
WO1998013445A1 (fr) * 1996-09-25 1998-04-02 Kelsan Technologies Corp. Lubrifiants solides et modificateurs de frottement pour les applications a lourdes charges et de chemin de fer
US6136757A (en) * 1996-09-25 2000-10-24 Kelsan Technologies Corporation Solid lubricants and friction modifiers for heavy loads and rail applications
AU736427B2 (en) * 1996-09-25 2001-07-26 Kelsan Technologies Corp. Solid lubricants and friction modifiers for heavy loads and rail applications
CZ297890B6 (cs) * 1996-09-25 2007-04-25 Kelsan Technologies Corp. Lubrikacní kompozice na vodném základu a kompozice pro modifikaci trení na vodném základu a jejich pouzití pro mazání kovového povrchu
EP1093510A1 (fr) * 1998-06-09 2001-04-25 Henkel Corporation Composition et procede pour l'enrobage de metaux avec un plastique lubrifie
US6455476B1 (en) 1998-06-09 2002-09-24 Henkel Corporation Composition and process for lubricated plastic working of metals
EP1093510A4 (fr) * 1998-06-09 2002-06-05 Henkel Corp Composition et procede pour l'enrobage de metaux avec un plastique lubrifie
WO2000043470A1 (fr) * 1999-01-22 2000-07-27 Nalco Chemical Company Composition a base d'eau pour usinage des metaux
WO2001098557A1 (fr) * 2000-06-21 2001-12-27 Henkel Kommanditgesellschaft Auf Aktien Agent adhesif dans des solutions pour conversion
WO2002020704A1 (fr) * 2000-09-05 2002-03-14 Honda Motor Co., Ltd. Agent lubrifiant aqueux de type a un stade pour forgeage a froid efficace
US8541350B2 (en) 2007-11-16 2013-09-24 Henkel Ag & Co. Kgaa Dry-film, anti-corrosive cold forming lubricant
US9192973B1 (en) 2013-03-13 2015-11-24 Meier Tool & Engineering, Inc. Drawing process for titanium
CN105014305A (zh) * 2014-04-21 2015-11-04 哈尔滨飞机工业集团有限责任公司 一种弯边的圆环形薄板的成形方法
CN108602670A (zh) * 2016-01-05 2018-09-28 纳米技术工业解决方案公司 水基纳米颗粒分散体
CN108602670B (zh) * 2016-01-05 2023-01-13 纳米技术工业解决方案公司 水基纳米颗粒分散体
CN109880681A (zh) * 2019-02-25 2019-06-14 江苏澳润新材料有限公司 一种超高温润滑脂添加剂及其制备方法
CN115612546A (zh) * 2020-06-03 2023-01-17 上海铂斯海特材料科技有限公司 一种水性金属冷挤压润滑剂及其制备工艺
CN113549912A (zh) * 2021-06-11 2021-10-26 河南航天精工制造有限公司 一种消除钛合金冷变形过程粘接性的润滑方法及化学硼化处理液

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JPH0368697A (ja) 1991-03-25
ES2048437T3 (es) 1994-03-16
JPH0747756B2 (ja) 1995-05-24
DE69005941T2 (de) 1994-05-19
DE69005941D1 (de) 1994-02-24
EP0412788B1 (fr) 1994-01-12

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