EP0711821A1 - Salt precoat as lubricant carrier for metal forming - Google Patents

Salt precoat as lubricant carrier for metal forming Download PDF

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Publication number
EP0711821A1
EP0711821A1 EP95115908A EP95115908A EP0711821A1 EP 0711821 A1 EP0711821 A1 EP 0711821A1 EP 95115908 A EP95115908 A EP 95115908A EP 95115908 A EP95115908 A EP 95115908A EP 0711821 A1 EP0711821 A1 EP 0711821A1
Authority
EP
European Patent Office
Prior art keywords
lubricant carrier
carrier salt
acid
weight
lubricant
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
EP95115908A
Other languages
German (de)
French (fr)
Other versions
EP0711821B1 (en
Inventor
Klaus-Dieter Nittel
Norbert Schwinke-Kruse
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.)
chemetal GmbH
Original Assignee
Metallgesellschaft AG
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Metallgesellschaft AG filed Critical Metallgesellschaft AG
Publication of EP0711821A1 publication Critical patent/EP0711821A1/en
Application granted granted Critical
Publication of EP0711821B1 publication Critical patent/EP0711821B1/en
Anticipated expiration legal-status Critical
Expired - Lifetime 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
    • C10M111/00—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential
    • C10M111/04—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential at least one of them being a macromolecular organic compound
    • 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
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    • C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
    • C—CHEMISTRY; METALLURGY
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    • C10M103/00—Lubricating compositions characterised by the base-material being an inorganic material
    • C10M103/06—Metal compounds
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    • C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
    • C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
    • C10M105/22—Carboxylic acids or their salts
    • C10M105/24—Carboxylic acids or their salts having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen
    • C—CHEMISTRY; METALLURGY
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    • C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
    • C10M105/22—Carboxylic acids or their salts
    • C10M105/26—Carboxylic acids or their salts having more than one carboxyl group bound to an acyclic carbon atom or cycloaliphatic carbon atom
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    • C10M107/36—Polysaccharides, e.g. cellulose
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    • C10M2201/0623—Oxides; Hydroxides; Carbonates or bicarbonates used as base material
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    • C10M2201/066—Molybdenum sulfide
    • C10M2201/0663—Molybdenum sulfide used as base material
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    • C10M2207/1253—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids used as base material
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/127—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic
    • C10M2207/1273—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids polycarboxylic used as base material
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/129—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/12—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/129—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms
    • C10M2207/1293—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of thirty or more carbon atoms used as base material
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/16—Naphthenic acids
    • C10M2207/163—Naphthenic acids used as base material
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/18—Tall oil acids
    • C10M2207/183—Tall oil acids used as base material
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/20—Rosin acids
    • C10M2207/203—Rosin acids used as base material
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/22—Acids obtained from polymerised unsaturated acids
    • C10M2207/223—Acids obtained from polymerised unsaturated acids used as base material
    • 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
    • C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10—Carboxylix acids; Neutral salts thereof
    • C10M2207/24—Epoxidised acids; Ester derivatives thereof
    • C10M2207/243—Epoxidised acids; Ester derivatives thereof used as base material
    • 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/12—Polysaccharides, e.g. cellulose, biopolymers
    • 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/12—Polysaccharides, e.g. cellulose, biopolymers
    • C10M2209/123—Polysaccharides, e.g. cellulose, biopolymers used as base material
    • 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
    • C10N2010/02—Groups 1 or 11

Definitions

  • the invention relates to a lubricant carrier salt to facilitate the cold forming of workpieces made of iron or steel based on boric acid and / or alkali borate, and to a method for facilitating the cold forming of workpieces made of iron or steel with the aid of this lubricant carrier salt.
  • fatty acid salts These are often applied to the workpieces to be formed in the form of hot, aqueous soap solutions.
  • a chemical coating is usually applied to the metal surface, e.g. a phosphate, oxide, oxalate or sulfide coating.
  • the lubricant should form a uniform film which forms a good separation layer between the workpiece and the tool during the forming treatment.
  • soaps In addition to the application of soaps to bare workpieces or workpieces that have previously been provided with a conversion coating, it is also known to use lubricants to facilitate cold forming represent a mixture of fatty acid salts and alkali pyrophosphate and / or alkali tetraborate (DE-A-1 594 512). Some of the soaps are said to be fatty acid salts of lithium, potassium, ammonium, calcium, mangesium, zinc and / or aluminum.
  • Lubricants are also known which contain neutral grease and / or oil, alkali metal soap and alkali metal salt of boric acid (DE-B-23 30 806), contain alkali borate, alkali sulfate and silicate as well as chloride (GB 1 561 836) or contain water-soluble metal soap , Alkali metal chloride, alkali metal sulfate and alkali metal borate (GB-A-2 003 923).
  • lubricant carrier salts are, for example, lime (Ca (OH) 2), iron hydroxide (Fe (OH) 2) and borax (Na2B4O7 ⁇ 10 H2O) (D. Oppen "Chemical surface treatment as a means to facilitate cold forming", Metall Structure (1982), pages 566 ff).
  • Borax in particular allows a high drawing speed.
  • its hygroscopicity is disadvantageous, so that the pullability, e.g. of the wire, falls off and rust formation is found on the wire surface.
  • the reason for the loss of traction is the decrease in liability associated with the increasing water absorption.
  • Another problem is the subsequent drying. E.g. the wire dries up, i.e. If the water of crystallization is wholly or only partially expelled from the borax applied, the borax layer loses its adhesion to the wire. The pulling ability is no longer given.
  • the object of the invention is a lubricant carrier salt to facilitate the cold forming of workpieces made of iron or steel based on boric acid and / or alkali borate
  • a lubricant carrier salt to facilitate the cold forming of workpieces made of iron or steel based on boric acid and / or alkali borate
  • the object is achieved by further developing the lubricant carrier salt of the type mentioned at the outset in accordance with the invention such that it contains aliphatic di- or tricarboxylic acid which is either unsubstituted or substituted by at least one OH group and / or an alkali salt thereof has, the weight ratio of boric acid / alkali borate (calculated as H3BO3) to carboxylic acid (calculated as citric acid) (5 to 15): 1.
  • di- or tricarboxylic acids are malonic acid, maleic acid, succinic acid, tartaric acid and / or citric acid.
  • carboxylic acids used in the lubricant carrier salt according to the invention should have a melting point above 100 ° C.
  • a further advantageous embodiment of the invention provides for the use of a lubricant carrier salt which contains an additional content of inorganic or organic thickener, preferably in amounts of 0.5 to 5% by weight on the fully formulated lubricant carrier salt).
  • Bentonite and / or polysaccharide are particularly suitable thickeners.
  • a further advantageous embodiment of the invention consists in applying a lubricant carrier salt which has an additional content of aluminate and / or silicate, preferably metasilicate and / or disilicate, in amounts of 1 to 10% by weight (based on the formulated lubricant carrier salt) .
  • a lubricant carrier salt which has an additional content of aluminate and / or silicate, preferably metasilicate and / or disilicate, in amounts of 1 to 10% by weight (based on the formulated lubricant carrier salt) .
  • a lubricant carrier salt which contains an additional content of dispersing, lubricating and / or rust inhibiting agents, preferably soap, in a total amount of 2 to 15% by weight (based on the formulated lubricant carrier salt) and / or an additional content of titanium salt, preferably of titanium phosphate, in amounts of 10 to 100 mg / kg of lubricant carrier salt (calculated as titanium).
  • the lubricant carrier salts according to the invention are usually applied to the workpieces in the form of an aqueous solution or dispersion. Accordingly, part of the invention is a method for facilitating the cold forming of workpieces made of iron or steel, which is characterized in that the lubricant carrier salt from an aqueous solution or dispersion with a concentration of 5 to 30 wt.% And at a temperature of 80 to 100 ° C is applied in a dipping or continuous process.
  • the lubricant carrier salt can be applied to the bare metal surface.
  • the invention is particularly suitable for wire drawing, cold upsetting, extrusion and ironing. Their particular advantages are that the lubricant carrier salt applied to the workpieces is insensitive to overdrying and shows practically no hygroscopic properties. The maximum water absorption after drying is 2% by weight.
  • a 15% by weight aqueous solution was prepared from the above-mentioned lubricant carrier salt, in which steel wire bundles were immersed for 10 minutes at a temperature of 90 ° C. Following the immersion treatment, drying was carried out at 150 ° C. in a forced air oven.
  • the steel wire had a lubricant carrier salt coating with a layer weight of 6 g / m2 due to the pretreatment mentioned.
  • the wire After applying soap before the drawing die, the wire, which had an initial diameter of 5.5 mm, was formed in eight passes at a drawing speed of 8 m / sec to a final diameter of 1.9 mm.
  • the basis weight of the phosphate coating produced with the phosphating solution was 10 g / m 2.
  • the lubricant carrier salt was applied from a 25% by weight solution heated to 90 ° C. in a continuous process, the contact time between steel wire and solution of the lubricant carrier salt being 15 seconds.
  • the lubricant carrier salt applied in this way had a weight of 4 g / m 2.
  • the steel wire was then shaped in six passes at 6 m / sec from the initial 6 mm to 3.5 mm after applying the soap. Here too, reproducible results were achieved with different storage times and partial overdrying.

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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)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Lubricants (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

Lubricant carrier salt is based on boric acid and/or alkali borate and contains aliphatic di- or tri-carboxylic acid (non)substd. by at least one OH group and their alkali salts The wt. ratio of boric acid/alkali borate (calc. as H3BO3) to carboxylic acid (calc. as citric acid) is 5-15:1. Also claimed is a process for facilitating cold forming of iron or steel workpieces, in which the lubricant carrier salt is applied as an aq. soln. or dispersion in a concn. of 5-30 wt. % and at 80-100 degrees C, to form a phosphate coating.

Description

Die Erfindung betrifft ein Schmiermittelträgersalz zur Erleichterung der Kaltumformung von Werkstücken aus Eisen oder Stahl auf Basis Borsäure und/oder Alkaliborat sowie ein Verfahren zur Erleichterung der Kaltumformung von Werkstücken aus Eisen oder Stahl mit Hilfe dieses Schmiermittelträgersalzes.The invention relates to a lubricant carrier salt to facilitate the cold forming of workpieces made of iron or steel based on boric acid and / or alkali borate, and to a method for facilitating the cold forming of workpieces made of iron or steel with the aid of this lubricant carrier salt.

Es ist bekannt, die Kaltumformung von metallischen Werkstücken durch Verwendung von fettsauren Salzen (Seifen) zu erleichtern. Diese werden häufig in Form heißer, wäßriger Seifenlösungen auf die umzuformenden Werkstücke aufgebracht. In manchen Fällen, insbesondere wenn schwere Verformungsoperationen durchgeführt werden sollen, pflegt man vor der Aufbringung des Schmiermittels einen chemischen Überzug auf die Metalloberfläche aufzubringen, z.B. einen Phosphat-, Oxid-, Oxalat- oder Sulfidüberzug. In beiden Fällen, d.h. bei Aufbringung des Schmiermittels auf das blanke Werkstück oder auf das zuvor mit einem chemischen Überzug versehene Werkstück, soll das Schmiermittel einen gleichmäßigen Film ausbilden, der eine gute Trennschicht zwischen Werkstück und Werkzeug während der Umformungsbehandlung bildet.It is known to facilitate the cold forming of metallic workpieces by using fatty acid salts (soaps). These are often applied to the workpieces to be formed in the form of hot, aqueous soap solutions. In some cases, especially when heavy deformation operations are to be performed, a chemical coating is usually applied to the metal surface, e.g. a phosphate, oxide, oxalate or sulfide coating. In both cases, i.e. when the lubricant is applied to the bare workpiece or to the workpiece previously provided with a chemical coating, the lubricant should form a uniform film which forms a good separation layer between the workpiece and the tool during the forming treatment.

Neben der Applikation von Seifen auf blanke oder zuvor mit einem Konversionsüberzug versehene Werkstücke ist es auch bekannt, Schmiermittel zur Erleichterung der Kaltumformung einzusetzen, die ein Gemisch aus fettsauren Salzen und Alkalipyrophosphat und/oder Alkalitetraborat darstellen (DE-A-1 594 512). Hierbei soll ein Teil der Seifen fettsaures Salz von Lithium, Kalium, Ammonium, Calcium, Mangesium, Zink und/oder Aluminium sein.In addition to the application of soaps to bare workpieces or workpieces that have previously been provided with a conversion coating, it is also known to use lubricants to facilitate cold forming represent a mixture of fatty acid salts and alkali pyrophosphate and / or alkali tetraborate (DE-A-1 594 512). Some of the soaps are said to be fatty acid salts of lithium, potassium, ammonium, calcium, mangesium, zinc and / or aluminum.

Auch sind Schmiermittel bekannt, die aus Neutralfett und/oder Öl, Alkalimetallseife sowie Alkalimetallsalz von Borsäure bestehen (DE-B-23 30 806), Alkaliborat, Alkalisulfat und Silikat sowie Chlorid enthalten (GB 1 561 836) oder aber einen Gehalt an wasserlöslicher Metallseife, Alkalimetallchlorid, Alkalimetallsulfat und Alkalimetallborat aufweisen (GB-A-2 003 923).Lubricants are also known which contain neutral grease and / or oil, alkali metal soap and alkali metal salt of boric acid (DE-B-23 30 806), contain alkali borate, alkali sulfate and silicate as well as chloride (GB 1 561 836) or contain water-soluble metal soap , Alkali metal chloride, alkali metal sulfate and alkali metal borate (GB-A-2 003 923).

Weiterhin ist es bekannt, auf metallische Werkstücke sogenannte Schmiermittelträgersalze aufzubringen, die selbst nicht als Schmiermittel wirken, sondern eine Nachbehandlung z.B. durch Beseifung an der Ziehmaschine erfahren. Derartige Schmiermittelträgersalze sind beispielsweise Kalk (Ca(OH)₂), Eisenhydroxid (Fe(OH)₂) und Borax (Na₂B₄O₇ · 10 H₂O) (D. Oppen "Chemische Oberflächenbehandlung als Mittel zur Erleichterung der Kaltumformung", Metalloberfläche (1982), Seiten 566 ff).Furthermore, it is known to apply so-called lubricant carrier salts to metallic workpieces, which do not themselves act as lubricants, but rather an aftertreatment, e.g. experienced by soaping on the drawing machine. Such lubricant carrier salts are, for example, lime (Ca (OH) ₂), iron hydroxide (Fe (OH) ₂) and borax (Na₂B₄O₇ · 10 H₂O) (D. Oppen "Chemical surface treatment as a means to facilitate cold forming", Metallfläche (1982), pages 566 ff).

Insbesondere Borax erlaubt zwar eine hohe Ziehgeschwindigkeit. Nachteilig ist jedoch seine Hygroskopizität, so daß die Ziehfähigkeit, z.B. des Drahtes, abfällt und eine Rostbildung auf der Drahtoberfläche festzustellen ist. Der Grund für den Verlust an Ziehfähigkeit ist der mit der steigenden Wasseraufnahme verbundene Abfall der Haftung. Ein weiteres Problem liegt in der anschließenden Trocknung. Wird z.B. der Draht übertrocknet, d.h. wird aus dem aufgebrachten Borax das Kristallwasser ganz oder auch nur teilweise ausgetrieben, verliert die Boraxschicht ihre Haftung zum Draht. Die Ziehfähigkeit ist damit nicht mehr gegeben.Borax in particular allows a high drawing speed. However, its hygroscopicity is disadvantageous, so that the pullability, e.g. of the wire, falls off and rust formation is found on the wire surface. The reason for the loss of traction is the decrease in liability associated with the increasing water absorption. Another problem is the subsequent drying. E.g. the wire dries up, i.e. If the water of crystallization is wholly or only partially expelled from the borax applied, the borax layer loses its adhesion to the wire. The pulling ability is no longer given.

Aufgabe der Erfindung ist es, ein Schmiermittelträgersalz zur Erleichterung der Kaltumformung von Werkstücken aus Eisen oder Stahl auf Basis Borsäure und/oder Alkaliborat bereitzustellen, das die Nachteile der bekannten Schmiermittelträgersalze nicht aufweist, insbesondere unempfindlich gegenüber dem Trockenprozeß ist und nach der Applikation nicht bzw. nur geringfügig hygroskopisch ist.The object of the invention is a lubricant carrier salt to facilitate the cold forming of workpieces made of iron or steel based on boric acid and / or alkali borate To provide, which does not have the disadvantages of the known lubricant carrier salts, is particularly insensitive to the drying process and is not or only slightly hygroscopic after application.

Die Aufgabe wird gelöst, indem das Schmiermittelträgersalz der eingangs genannten Art entsprechend der Erfindung derart weitergebildet wird, daß es einen Gehalt an aliphatischer Di- oder Tricarbonsäure, die entweder nicht substituiert oder durch mindestens eine OH-Gruppe substituiert ist, und/oder ein Alkalisalz hiervon aufweist, wobei das Gewichtsverhältnis von Borsäure/Alkaliborat (berechnet als H₃BO₃) zu Carbonsäure (berechnet als Zitronensäure) (5 bis 15) : 1 beträgt.The object is achieved by further developing the lubricant carrier salt of the type mentioned at the outset in accordance with the invention such that it contains aliphatic di- or tricarboxylic acid which is either unsubstituted or substituted by at least one OH group and / or an alkali salt thereof has, the weight ratio of boric acid / alkali borate (calculated as H₃BO₃) to carboxylic acid (calculated as citric acid) (5 to 15): 1.

Die vorstehend verwendete Formulierung "aliphatische Di- oder Tricarbonsäure, die entweder nicht substituiert oder durch mindestens eine OH-Gruppe substituiert ist" bedeutet, daß die verwendete Carbonsäure mindestens eine substituierbare CH₂- oder CH-Gruppe aufweisen muß.The formulation used above "aliphatic di- or tricarboxylic acid which is either unsubstituted or substituted by at least one OH group" means that the carboxylic acid used must have at least one substitutable CH₂ or CH group.

Besonders geeignete Di- bzw. Tricarbonsäuren sind Malonsäure, Maleinsäure, Bernsteinsäure, Weinsäure und/oder Zitronensäure. Insbesondere sollten die im erfindungsgemäßen Schmiermittelträgersalz zum Einsatz gelangenden Carbonsäuren einen Schmelzpunkt oberhalb 100°C aufweisen.Particularly suitable di- or tricarboxylic acids are malonic acid, maleic acid, succinic acid, tartaric acid and / or citric acid. In particular, the carboxylic acids used in the lubricant carrier salt according to the invention should have a melting point above 100 ° C.

Um die Filmdicke des aufgebrachten Schmiermittelträgersalzes innerhalb bestimmter Grenzen einstellen zu können, sieht eine weitere vorteilhafte Ausgestaltung der Erfindung vor, ein Schmiermittelträgersalz einzusetzen, das einen zusätzlichen Gehalt an anorganischem oder organischem Verdickungsmittel, vorzugsweise in Mengen von 0,5 bis 5 Gew.% (bezogen auf das fertig formulierte Schmiermittelträgersalz), aufweist. Besonders geeignete Verdickungsmittel sind Bentonit und/oder Polysaccharid.In order to be able to adjust the film thickness of the applied lubricant carrier salt within certain limits, a further advantageous embodiment of the invention provides for the use of a lubricant carrier salt which contains an additional content of inorganic or organic thickener, preferably in amounts of 0.5 to 5% by weight on the fully formulated lubricant carrier salt). Bentonite and / or polysaccharide are particularly suitable thickeners.

Eine weitere vorteilhafte Ausgestaltung der Erfindung besteht darin, ein Schmiermittelträgersalz aufzubringen, das einen zusätzlichen Gehalt an Aluminat und/oder Silikat, vorzugsweise von Metasilikat und/oder Disilikat, in Mengen von 1 bis 10 Gew.% (bezogen auf das fertig formulierte Schmiermittelträgersalz) aufweist. Hierdurch wird erreicht, daß das auf das Werkstück aufgebrachte Schmiermittelträgersalz eine definierte Rauhigkeit erhält und damit eine definierte Schmiermittelmenge in das Umformungswerkzeug transportiert.A further advantageous embodiment of the invention consists in applying a lubricant carrier salt which has an additional content of aluminate and / or silicate, preferably metasilicate and / or disilicate, in amounts of 1 to 10% by weight (based on the formulated lubricant carrier salt) . This ensures that the lubricant carrier salt applied to the workpiece receives a defined roughness and thus transports a defined amount of lubricant into the forming tool.

Schließlich ist es von Vorteil, auf die Werkstücke ein Schmiermittelträgersalz zu applizieren, das einen zusätzlichen Gehalt an Dispergier-, Gleit- und/oder Rostschutzmitteln, vorzugsweise Seife, in einer Gesamtmenge von 2 bis 15 Gew.% (bezogen auf das fertig formulierte Schmiermittelträgersalz) und/oder einen zusätzlichen Gehalt an Titansalz, vorzugsweise an Titanphosphat, in Mengen von 10 bis 100 mg/kg Schmiermittelträgersalz (berechnet als Titan) besitzt. Die besonderen Vorzüge derartiger Zusätze bestehen darin, daß der Kontakt Werkstück/Werkzeug besonders effektiv verhindert wird.Finally, it is advantageous to apply a lubricant carrier salt to the workpieces, which contains an additional content of dispersing, lubricating and / or rust inhibiting agents, preferably soap, in a total amount of 2 to 15% by weight (based on the formulated lubricant carrier salt) and / or an additional content of titanium salt, preferably of titanium phosphate, in amounts of 10 to 100 mg / kg of lubricant carrier salt (calculated as titanium). The particular advantages of such additives are that the workpiece / tool contact is prevented particularly effectively.

Die erfindungsgemäßen Schmiermittelträgersalze werden üblicherweise in Form einer wäßrigen Lösung oder Dispersion auf die Werkstücke aufgebracht. Demzufolge ist Bestandteil der Erfindung ein Verfahren zur Erleichterung der Kaltumformung von Werkstücken aus Eisen oder Stahl, das dadurch gekennzeichnet ist, daß das Schmiermittelträgersalz aus einer wäßrigen Lösung oder Dispersion mit einer Konzentration von 5 bis 30 Gew.% und mit einer Temperatur von 80 bis 100°C im Tauchen oder Durchlaufverfahren aufgebracht wird.The lubricant carrier salts according to the invention are usually applied to the workpieces in the form of an aqueous solution or dispersion. Accordingly, part of the invention is a method for facilitating the cold forming of workpieces made of iron or steel, which is characterized in that the lubricant carrier salt from an aqueous solution or dispersion with a concentration of 5 to 30 wt.% And at a temperature of 80 to 100 ° C is applied in a dipping or continuous process.

Die Applikation des Schmiermittelträgersalzes kann auf die blanke Metalloberfläche erfolgen. Besonders zweckmäßig ist es jedoch entsprechend einer weiteren vorteilhaften Ausgestaltung des erfindungsgemäßen Verfahrens, vor der Aufbringung das Schmiermittelträgersalzes die Werkstücke aus Eisen oder Stahl mit einem Phosphatüberzug zu versehen. Hierdurch wird z.B. bei Mehrfachzügen ein Kontakt zwischen Werkstück und Werkzeug wirksam verhindert.The lubricant carrier salt can be applied to the bare metal surface. However, according to a further advantageous embodiment of the method according to the invention, it is particularly expedient to provide the iron or steel workpieces with a phosphate coating before the lubricant carrier salt is applied. This will, for example, at Multiple moves effectively prevent contact between workpiece and tool.

Die Erfindung eignet sich insbesondere zum Drahtzug, zum Kaltstauchen, zum Fließpressen und zum Abstreckziehen. Ihre besonderen Vorzüge liegen darin, daß das auf die Werkstücke aufgebrachte Schmiermittelträgersalz unempfindlich gegenüber einer Übertrocknung ist und praktisch keine hygroskopischen Eigenschaften zeigt. Die maximale Wasseraufnahme nach der erfolgten Trocknung beträgt 2 Gew.%.The invention is particularly suitable for wire drawing, cold upsetting, extrusion and ironing. Their particular advantages are that the lubricant carrier salt applied to the workpieces is insensitive to overdrying and shows practically no hygroscopic properties. The maximum water absorption after drying is 2% by weight.

Die Erfindung wird anhand der nachfolgenden Beispiele beispielsweise und näher erläutert.The invention is illustrated by the following examples, for example and in more detail.

Beispiel 1example 1

Zum Einsatz gelangte ein Schmiermittelträgersalz, das folgende Bestandteile aufwies:

50
Gew.% Borsäure (H₃BO₃)
15
Gew.% Kaliumborat (K₂B₄O₇·4H₂O)
10
Gew.% Natriumborat (Neobor, Na₂B₄O₇·5H₂O)
5
Gew.% Natriumdisilikat (Na₂Si₂O₅·xH₂O)
10
Gew.% Zitronensäure
10
Gew.% Natriumstearat.
A lubricant carrier salt was used, which had the following components:
50
% By weight boric acid (H₃BO₃)
15
% By weight potassium borate (K₂B₄O₇4H₂O)
10th
% By weight sodium borate (Neobor, Na₂B₄O₇ · 5H₂O)
5
% By weight sodium disilicate (Na₂Si₂O₅ · xH₂O)
10th
% By weight citric acid
10th
% By weight sodium stearate.

Aus dem vorstehend genannten Schmiermittelträgersalz wurde eine 15 Gew.%ige wäßrige Lösung hergestellt, in der Bunde aus Stahldraht bei einer Temperatur von 90°C 10 min im Tauchen behandelt wurden. Im Anschluß an die Tauchbehandlung erfolgte eine Trocknung bei 150°C im Umluftofen. Der Stahldraht hatte aufgrund der genannten Vorbehandlung eine Schmiermittelträgersalzauflage mit einem Schichtgewicht von 6 g/m². Nach dem Auftrag von Seife vor dem Ziehstein wurde der Draht, der einen anfänglichen Durchmesser von 5,5 mm hatte, in acht Zügen mit einer Ziehgeschwindigkeit von 8 m/sec auf einen Enddurchmesser von 1,9 mm umgeformt. Diese Ergebnisse wurden bei wechselnden Lagerzeiten des mit dem Schmiermittelträgersalz beschichteten Drahtes und teilweiser Übertrocknung reproduzierbar erreicht.A 15% by weight aqueous solution was prepared from the above-mentioned lubricant carrier salt, in which steel wire bundles were immersed for 10 minutes at a temperature of 90 ° C. Following the immersion treatment, drying was carried out at 150 ° C. in a forced air oven. The steel wire had a lubricant carrier salt coating with a layer weight of 6 g / m² due to the pretreatment mentioned. After applying soap before the drawing die, the wire, which had an initial diameter of 5.5 mm, was formed in eight passes at a drawing speed of 8 m / sec to a final diameter of 1.9 mm. These results have been changing Storage times of the wire coated with the lubricant carrier salt and partial overdrying reproducibly achieved.

Beispiel 2Example 2

Zur Vorbereitung von ebenfalls Stahldrähten wurde ein Schmiermittelträgersalz eingesetzt, das folgende Bestandteile enthielt:

40
Gew.% Borsäure (H₃BO₃)
35
Gew.% Kaliumborat (K₂B₄O₇·4H₂O)
2,9
Gew.% Natriumdisilikat (Na₂Si₂O₅·xH₂O)
10
Gew.% Zitronensäure
0,1
Gew.% Titanylsulfat
5
Gew.% Polysaccharid
7
Gew.% Kaliumoleat.
A lubricant carrier salt was used to prepare steel wires, which contained the following components:
40
% By weight boric acid (H₃BO₃)
35
% By weight potassium borate (K₂B₄O₇4H₂O)
2.9
% By weight sodium disilicate (Na₂Si₂O₅ · xH₂O)
10th
% By weight citric acid
0.1
% By weight of titanyl sulfate
5
% By weight of polysaccharide
7
% By weight potassium oleate.

Vor der Aufbringung des Schmiermittelträgersalzes war der Stahldraht im Tauchen mit Hilfe von Salzsäure von Rost und Zunder befreit und nach gründlicher Wasserspülung 6 bis 10 min bei 45°C phosphatiert worden. Die Zusammensetzung der Phosphatierungslösung betrug:

10,9
g/l Zink,
2,1
g/l Mangan,
2,0
g/l Eisen(II),
0,5
g/l Calcium,
0,5
g/l Nickel,
0,01
g/l Kupfer,
0,3
g/l Natrium,
24,0
g/l Nitrat,
10,6
g/l Phosphat (berechnet als P₂O₅),
1,6
g/l Tetrafluoroborat,
1,6
g/l Weinsäure und
0,5
g/l Harnstoff.
Before the lubricant carrier salt was applied, the steel wire was freed of rust and scale by dipping with hydrochloric acid and phosphated at 45 ° C. for 6 to 10 minutes after thorough water rinsing. The composition of the phosphating solution was:
10.9
g / l zinc,
2.1
g / l manganese,
2.0
g / l iron (II),
0.5
g / l calcium,
0.5
g / l nickel,
0.01
g / l copper,
0.3
g / l sodium,
24.0
g / l nitrate,
10.6
g / l phosphate (calculated as P₂O₅),
1.6
g / l tetrafluoroborate,
1.6
g / l tartaric acid and
0.5
g / l urea.

Das mit der Phosphatierungslösung erzeugte Flächengewicht des Phosphatüberzuges betrug 10 g/m².The basis weight of the phosphate coating produced with the phosphating solution was 10 g / m 2.

Die Applikation des Schmiermittelträgersalzes erfolgte aus einer 25 Gew.%igen, auf 90°C erwärmten Lösung im Durchlaufverfahren, wobei die Kontaktdauer zwischen Stahldraht und Lösung des Schmiermittelträgersalzes 15 sec betrug. Das auf diese Weise aufgebrachte Schmiermittelträgersalz hatte ein Gewicht von 4 g/m².The lubricant carrier salt was applied from a 25% by weight solution heated to 90 ° C. in a continuous process, the contact time between steel wire and solution of the lubricant carrier salt being 15 seconds. The lubricant carrier salt applied in this way had a weight of 4 g / m 2.

Anschließend wurde der Stahldraht nach Seifenauftrag vor dem Ziehstein in sechs Zügen mit 6 m/sec von anfänglich 6 mm auf 3,5 mm umgeformt. Auch hier wurden bei unterschiedlichen Lagerzeiten und teilweiser Übertrocknung reproduzierbare Ergebnisse erzielt.The steel wire was then shaped in six passes at 6 m / sec from the initial 6 mm to 3.5 mm after applying the soap. Here too, reproducible results were achieved with different storage times and partial overdrying.

Claims (9)

Schmiermittelträgersalz zur Erleichterung der Kaltumformung von Werkstücken aus Eisen oder Stahl auf Basis Borsäure und/oder Alkaliborat, gekennzeichnet durch einen Gehalt an aliphatischer Di- oder Tricarbonsäure, die entweder nicht substituiert oder durch mindestens eine OH-Gruppe substituiert ist, und/oder an Alkalisalzen hiervon, wobei das Gewichtsverhältnis von Borsäure/Alkaliborat (berechnet als H₃BO₃) zu Carbonsäure (berechnet als Zitronensäure) (5 bis 15) : 1 beträgt.Lubricant carrier salt to facilitate the cold forming of workpieces made of iron or steel based on boric acid and / or alkali borate, characterized by a content of aliphatic di- or tricarboxylic acid, which is either unsubstituted or substituted by at least one OH group, and / or alkali salts thereof , wherein the weight ratio of boric acid / alkali borate (calculated as H₃BO₃) to carboxylic acid (calculated as citric acid) (5 to 15): 1. Schmiermittelträgersalz nach Anspruch 1, gekennzeichnet durch einen Gehalt an Malonsäure, Maleinsäure, Bernsteinsäure, Weinsäure und/oder Zitronensäure.Lubricant carrier salt according to claim 1, characterized by a content of malonic acid, maleic acid, succinic acid, tartaric acid and / or citric acid. Schmiermittelträgersalz nach Anspruch 1 oder 2, gekennzeichnet durch einen zusätzlichen Gehalt an anorganischem oder organischem Verdickungsmittel, vorzugsweise in Mengen von 0,5 bis 5 Gew.% (bezogen auf das fertig formulierte Schmiermittelträgersalz).Lubricant carrier salt according to claim 1 or 2, characterized by an additional content of inorganic or organic thickener, preferably in amounts of 0.5 to 5% by weight (based on the formulated lubricant carrier salt). Schmiermittelträgersalz nach Anspruch 3, gekennzeichnet durch einen Gehalt an Bentonit und/oder Polysaccharid als Verdickungsmittel.Lubricant carrier salt according to claim 3, characterized by a content of bentonite and / or polysaccharide as a thickener. Schmiermittelträgersalz nach einem oder mehreren der Ansprüche 1 bis 4, gekennzeichnet durch einen zusätzlichen Gehalt an Aluminat und/oder Silikat, vorzugsweise Metasilikat und/oder Disilikat, in Mengen von 1 bis 10 Gew.% (bezogen auf das fertig formulierte Schmiermittelträgersalz).Lubricant carrier salt according to one or more of claims 1 to 4, characterized by an additional content of aluminate and / or silicate, preferably metasilicate and / or disilicate, in amounts of 1 to 10% by weight (based on the formulated lubricant carrier salt). Schmiermittelträgersalz nach einem oder mehreren der Ansprüche 1 bis 5, gekennzeichnet durch einen zusätzlichen Gehalt an Dispergier-, Gleit- und/oder Rostschutzmitteln, vorzugsweise an Seife, in einer Gesamtmenge von 2 bis 15 Gew.% (bezogen auf das fertig formulierte Schmiermittelträgersalz).Lubricant carrier salt according to one or more of claims 1 to 5, characterized by an additional content of dispersants, lubricants and / or rust inhibitors, preferably soap, in a total amount of 2 to 15% by weight (based on the formulated lubricant carrier salt). Schmiermittelträgersalz nach einem oder mehreren der Ansprüche 1 bis 6, gekennzeichnet durch einen zusätzlichen Gehalt an Titansalz, vorzugsweise an Titanphosphat, in Mengen von 10 bis 100 mg/kg Schmiermittelträgersalz (berechnet als Titan).Lubricant carrier salt according to one or more of claims 1 to 6, characterized by an additional content of titanium salt, preferably titanium phosphate, in amounts of 10 to 100 mg / kg of lubricant carrier salt (calculated as titanium). Verfahren zur Erleichterung der Kaltumformung von Werkstücken aus Eisen oder Stahl, dadurch gekennzeichnet, daß das Schmiermittelträgersalz gemäß einem oder mehreren der Ansprüche 1 bis 7 aus einer wäßrigen Lösung oder Dispersion mit einer Konzentration von 5 bis 30 Gew.% und mit einer Temperatur von 80 bis 100°C im Tauchen oder Durchlaufverfahren aufgebracht wird.Process for facilitating the cold forming of workpieces made of iron or steel, characterized in that the lubricant carrier salt according to one or more of claims 1 to 7 from an aqueous solution or dispersion with a concentration of 5 to 30% by weight and at a temperature of 80 to 100 ° C is applied by dipping or continuous process. Verfahren nach Anspruch 8, dadurch gekennzeichnet, daß auf den Werkstücken aus Eisen oder Stahl vor der Aufbringung des Schmiermittelträgersalzes ein Phosphatüberzug erzeugt wird.Method according to Claim 8, characterized in that a phosphate coating is produced on the workpieces made of iron or steel before the lubricant carrier salt is applied.
EP95115908A 1994-11-11 1995-10-10 Salt precoat as lubricant carrier for metal forming Expired - Lifetime EP0711821B1 (en)

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DE4440301 1994-11-11
DE4440301A DE4440301A1 (en) 1994-11-11 1994-11-11 Lubricant carrier salt for metal forming

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WO2009095375A1 (en) * 2008-01-30 2009-08-06 Chemetall Gmbh Method for coating metal surfaces with a lubricant composition
WO2009095374A1 (en) 2008-01-30 2009-08-06 Chemetall Gmbh Method for coating metal surfaces with a wax-containing lubricant composition
WO2009095373A1 (en) 2008-01-30 2009-08-06 Chemetall Gmbh Method for coating metal surfaces with a phosphate layer and then with a polymer lubricant layer
IT202200006158A1 (en) 2022-03-29 2023-09-29 Condoroil Chemical S R L PROCESS TO PRODUCE A BORON-FREE COLD DEFORMATION COATING

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AU6212000A (en) * 1999-07-13 2001-01-30 Century Chemical Corporation Improved process and product for lubricating metal prior to cold forming
JPWO2002020704A1 (en) * 2000-09-05 2004-01-15 本田技研工業株式会社 Water-based one-step type lubricant for high efficiency cold forging
AU2003286655A1 (en) * 2002-10-25 2004-05-13 University Of Chicago Improved metalworking and machining fluids
WO2007116653A1 (en) * 2006-03-27 2007-10-18 Sumitomo Metal Industries, Ltd. Lubricant for hot plastic working and powder lubricant composition for hot working
CN114317077A (en) * 2021-12-23 2022-04-12 南京华舜润滑制品有限公司 Production process of wire-drawing lubricating powder

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WO2009095375A1 (en) * 2008-01-30 2009-08-06 Chemetall Gmbh Method for coating metal surfaces with a lubricant composition
WO2009095374A1 (en) 2008-01-30 2009-08-06 Chemetall Gmbh Method for coating metal surfaces with a wax-containing lubricant composition
WO2009095373A1 (en) 2008-01-30 2009-08-06 Chemetall Gmbh Method for coating metal surfaces with a phosphate layer and then with a polymer lubricant layer
AU2009209697B2 (en) * 2008-01-30 2013-02-07 Chemetall Gmbh Method for coating metal surfaces with a phosphate layer and then with a polymer lubricant layer
US8915108B2 (en) 2008-01-30 2014-12-23 Chemetall Gmbh Method for coating metal surfaces with a lubricant composition
US8956699B2 (en) 2008-01-30 2015-02-17 Chemetall Gmbh Method for coating metal surfaces with a wax-containing lubricant composition
US9422503B2 (en) 2008-01-30 2016-08-23 Chemetall Gmbh Method for coating metal surfaces with a phosphate layer and then with a polymer lubricant layer
IT202200006158A1 (en) 2022-03-29 2023-09-29 Condoroil Chemical S R L PROCESS TO PRODUCE A BORON-FREE COLD DEFORMATION COATING

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DE4440301A1 (en) 1996-05-15
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US5584945A (en) 1996-12-17
ATE193049T1 (en) 2000-06-15
ES2148394T3 (en) 2000-10-16

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