CN111771014A - Metal material for plastic working - Google Patents

Metal material for plastic working Download PDF

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Publication number
CN111771014A
CN111771014A CN201980014024.3A CN201980014024A CN111771014A CN 111771014 A CN111771014 A CN 111771014A CN 201980014024 A CN201980014024 A CN 201980014024A CN 111771014 A CN111771014 A CN 111771014A
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CN
China
Prior art keywords
film
metal material
acid
coating
plastic working
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Pending
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CN201980014024.3A
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Chinese (zh)
Inventor
冈田康宏
柳睦
青山充
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.)
Japan Pakase Seiki Co ltd
Nihon Parkerizing Co Ltd
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Japan Pakase Seiki Co ltd
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Application filed by Japan Pakase Seiki Co ltd filed Critical Japan Pakase Seiki Co ltd
Priority to CN202310185445.0A priority Critical patent/CN116200733A/en
Publication of CN111771014A publication Critical patent/CN111771014A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different 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
    • 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
    • C10M105/28—Carboxylic acids or their salts having only one carboxyl group bound to a carbon atom of a six-membered aromatic ring
    • 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
    • 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
    • C10M105/30—Carboxylic acids or their salts having more than one carboxyl group bound to a carbon atom of a six-membered aromatic ring
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
    • C23C22/08—Orthophosphates
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/46—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing oxalates
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/78—Pretreatment of the material to be coated
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/82—After-treatment
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23C26/00—Coating not provided for in groups C23C2/00 - C23C24/00

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Laminated Bodies (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Lubricants (AREA)

Abstract

The technical problem of the present invention is to provide a metal material for plastic working having excellent welding resistance. The above-described problems can be solved by a metal material for plastic working according to the present invention, which has a1 st film on a surface of a metal material, and a2 nd film on a surface of the 1 st film, wherein the 2 nd film is a surface layer, and the 2 nd film contains a compound having a benzene ring directly bonded to at least 1 carboxyl group, or a salt thereof, or a peroxide thereof.

Description

Metal material for plastic working
Technical Field
The present invention relates to a metal material for plastic working, which has a coating film required for plastic working such as forging (including cold, warm, hot forging), wire drawing, and pipe drawing of a steel material or another metal material.
Background
In plastic working of a metal material, a mold and the metal material for plastic working may be welded together. Not only the intended molded product cannot be obtained by the fusion welding, but also the size of the mold is changed by the influence of the metal to be fused, and the number of times the mold can be used is shortened. Therefore, the mold has to be remanufactured, resulting in a reduction in cost efficiency. Therefore, a metal material for plastic working excellent in weld resistance is required.
For example, patent document 1 discloses a lubricant for thermoplastic processing and thermoplastic processing, which contains an alkali metal salt of an aromatic carboxylic acid compound having 2 or more carboxyl groups, several kinds of water-soluble polymer compounds, and water.
Patent document 2 discloses a lubricant for warm forging and hot forging, which contains a specific compound obtained by bonding 2 aromatic rings having 2 carboxyl groups located at the ortho-position.
Patent document 3 discloses a lubricant composition for aqueous cold plastic working, which contains an aromatic carboxylic acid salt having a melting point of 90 ℃ or higher, which is composed of sodium hydroxide or potassium hydroxide, a water-soluble polymer compound and/or wax, and water.
Documents of the prior art
Patent document
Patent document 1: japanese patent laid-open publication No. 2015-89938;
patent document 2: japanese laid-open patent publication No. 2015-89939;
patent document 3: japanese patent laid-open publication No. 2015-17171.
Disclosure of Invention
Problems to be solved by the invention
The invention aims to provide a metal material for plastic working with excellent welding resistance.
Means for solving the problems
As a result of intensive studies to solve the above problems, the present inventors have found that a metal material for plastic working having excellent fusion welding resistance has a1 st film on the surface or surface of the metal material, a2 nd film on the surface or surface of the 1 st film, the 2 nd film being a surface layer, and the 2 nd film containing a compound having a benzene ring directly bonded to at least 1 carboxyl group or a salt thereof, or a peroxide thereof, and have completed the present invention.
The invention (1) is a metal material for plastic working,
which has a1 st film on the surface of a metal material,
a2 nd coating film on the surface or on the surface of the 1 st coating film,
the 2 nd coating film is a surface layer,
the 2 nd film contains a compound having a benzene ring directly bonded to at least 1 carboxyl group, a salt thereof, or a peroxide thereof.
Effects of the invention
According to the present invention, it is possible to provide a metal material for plastic working which is excellent in the effect of preventing fusion welding (fusion welding resistance) due to friction between a die and the metal material for forming working which occurs during plastic working.
Drawings
Fig. 1 is a view showing the evaluation criteria of fusion welding resistance of test pieces subjected to the workability evaluation test (photograph is used as a drawing).
Detailed Description
The present invention will be described in detail below.
< Metal Material for Plastic working >
A metal material for plastic working according to an embodiment of the present invention includes: the metal material, 1 st coating on the surface or surface of the metal material, and 2 nd coating on the surface or surface of the 1 st coating, the 2 nd coating contains a compound having a benzene ring directly bonded to at least 1 carboxyl group, a salt thereof, or a peroxide thereof. Further, a single layer or a plurality of layers of the film may be provided between the 1 st film and the 2 nd film, and the 2 nd film may be present in the surface layer.
The plastic working in the present specification is not particularly limited as long as it is a known plastic working, and examples thereof include: forging (cold, warm, hot), extrusion, wire drawing, tube drawing, crimping, bending, joining, shearing, shaping, and the like. Among them, the metal material for plastic working of the present invention is preferably used for plastic working in which a load applied to the metal material is particularly large, such as forging, wire drawing and pipe drawing.
1. Constitution of metal material for plastic working
1-1. metallic Material
The metal material is not particularly limited, and is generally a metal material used for plastic working. Examples thereof include: iron, iron alloys (steel, stainless steel, etc.), aluminum alloys, magnesium alloys, titanium alloys, copper alloys, tin alloys, zinc alloys, and the like.
The metal material may be a plating material having a plating film as long as the effects of the present invention are not impaired. The material of the plating film is not particularly limited, and for example: a metal such as nickel, iron, aluminum, manganese, chromium, magnesium, cobalt, lead, zinc, tin, or antimony, or an alloy of a plurality of metals, and a metal or an alloy of a plurality of metals containing unavoidable impurities can be used.
In the case of artificially forming a plating film, a known method can be used for the formation method, and examples thereof include: electro plating (electrolytic plating, electroplating), electroless plating, hot dip plating, vapor phase plating, mechanical plating, thermal spraying, and the like.
The thickness of the plating film is not particularly limited, and is, for example, 0.1 μm or more and 1000 μm or less.
Further, an oxide film may be formed on the surface of the metal material. The oxide film is not particularly limited, and may be a natural oxide film naturally occurring in the atmosphere or an artificially formed oxide film.
The method for forming the artificial oxide film is not particularly limited, and examples thereof include: a method of anodizing by electrifying a metal material as an anode in an electrolyte solution, a method of immersing in a strongly acidic liquid, a method using electropolishing, a method using plasma electrolysis, and the like. The oxide film may be subjected to sealing treatment by a steam method, a pure water boiling water method, a nickel acetate method, a dichromic acid method, a sodium silicate method, or the like.
The thickness of the oxide film is not particularly limited, and is, for example, 0.001 μm or more and 100 μm or less.
The shape of the metal material is not limited to a bar-like material, a block-like material, or other blank shape, and may be a machined shape (gear, shaft, or the like), and is not particularly limited.
1-2. the No. 1 skin film
The 1 st film is not particularly limited, and for example, a chemically synthesized film, a coating film, or the like can be used.
1-2-1. chemical synthesis of skin membrane
An example of a mechanism of film deposition in the chemical synthesis treatment is as follows. When the metallic material is brought into contact with the chemical synthesis treatment agent,h in which the surface of a metal material is treated with an acid component (etching component) in a chemical synthesis treatment agent+The ion etching (dissolution) causes the pH near the surface to rise. As the pH near the surface rises, the etched metal components in the metal material present near the surface and the components contained in the chemical synthesis treatment solution are precipitated as insoluble salts on the surface of the metal material. The insoluble salt forms a film.
The chemical synthesis coating is not particularly limited, and is composed of, for example, a phosphate, an oxalate, an aluminate, a chromate, a molybdate, a zirconium compound, a titanium compound, a vanadium compound, a hafnium compound, and the like. In addition, they may be composed of a single salt or may be composed of a plurality of salts. The chemical synthesis coating is preferably formed of phosphate, oxalate, or aluminate, and more preferably formed of zinc phosphate or iron oxalate.
The phosphate is not particularly limited, and examples thereof include: zinc phosphate, zinc iron phosphate, nickel phosphate, manganese phosphate, iron manganese phosphate, calcium phosphate, cobalt phosphate, magnesium phosphate, aluminum phosphate, sodium phosphate, potassium phosphate, ammonium phosphate, and the like. When the metal material is steel, stainless steel, or the like, the phosphate is preferable.
The oxalate is not particularly limited, and examples thereof include: sodium oxalate, potassium oxalate, ferric oxalate, ammonium oxalate and the like. In the case where the metal material is stainless steel or the like, the oxalate is preferable.
The aluminate is not particularly limited, and examples thereof include: lithium aluminate, sodium aluminate, potassium aluminate, magnesium aluminate, calcium aluminate, and the like. In the case where the metal material is aluminum or an aluminum alloy, the aluminate is preferable.
The amount of the above-mentioned chemically synthesized coating is not particularly limited, but is, for example, 0.5g/m2Above and 20.0g/m2Hereinafter, it is preferably 2.0g/m2Above and 10.0g/m2The following. The amount of the above-mentioned deposited substance can be adjusted by changing the composition, concentration, etc. of the chemical synthesis treatment agent, or by changing the contact conditions such as the contact method, contact temperature, contact time, etc.
1-2-2. coating film
The coating film is a film formed by applying a coating film agent to the surface of a metal material.
The material of the coating film is not particularly limited, and any material may be used as long as it can be formed on the surface or the surface of the metal material of the present embodiment and can form the 2 nd coating film on the surface or the surface. Examples of the coating film formed by using the coating type coating agent include: a coating film formed by a coating chromate treatment with a treatment liquid containing chromic acid, dichromic acid, or a salt thereof as a main component; a coating film formed by a coating-type chromate-free treatment not involving chromic acid or dichromic acid; a coating film formed from a silane coupling agent monomer; silica, silica colloid, and the like, which are modified with a silane coupling agent and the like; an organic resin film containing an urethane resin, an epoxy resin, an acrylic resin, an olefin resin such as polyethylene, polypropylene, or an ethylene-acrylic acid copolymer, a styrene resin such as polystyrene, a polyester, or a copolymer or modified product thereof; inorganic films (except for plating films and oxide films) containing glass such as lithium silicate and sodium silicate, metal oxysalts, metal hydroxides, metal phosphates, metal fluoride compounds, and the like; and a coating film obtained by dispersing a lubricant in a solvent such as water or oil or a base polymer such as a copolymer of styrene and maleic acid/maleic anhydride.
The solid lubricant is not particularly limited, and examples thereof include: waxes such as polyethylene wax and polypropylene wax; layered clay minerals such as montmorillonite, vermiculite, mica, brittle mica, pyrophyllite, and kaolinite; polytetrafluoroethylene; fatty acid metal soaps, fatty acid amides; molybdenum disulfide; tungsten disulfide; graphite; and melamine cyanurate and the like.
1-3. 2 nd skin film
1-3-1. material quality
The 2 nd coating of the present embodiment includes at least one or more of the following: a compound having a benzene ring directly bonded to at least 1 carboxyl group in the structure, or a salt thereof, or a peroxide thereof. In the present specification, a compound having a benzene ring directly bonded to at least 1 carboxyl group is sometimes described as an aromatic carboxylic acid compound.
The benzene ring in the present invention refers to a compound having 1 benzene ring alone, such as a benzene compound, but is not limited thereto, and includes a condensed polycyclic aromatic hydrocarbon in which a plurality of benzene rings are directly condensed, such as naphthalene or anthracene.
The aromatic carboxylic acid compound is not particularly limited as long as the effects of the present invention are not impaired, and examples thereof include: pyrogalloic acid, xylylic acid, mellitic acid, trimesic acid (mesitylene acid), 2,3, 4-trimethylbenzoic acid (prenylic acid), duronic acid (durylic acid), beta-isoduronic acid, alpha-isoduronic acid, anisic acid, o-methylsalicylic acid (o-cresylic acid), m-methylsalicylic acid, p-methylsalicylic acid, o-pyrocatechoic acid, beta-resorcylic acid, gentisic acid, gamma-resorcylic acid, protocatechuic acid, alpha-resorcylic acid, vanillic acid, isovanillic acid, veratric acid, 2, 3-dimethoxybenzoic acid, glycosidic acid, m-hemipinac acid, gallic acid, syringic acid, caprylic acid (asaronic acid), homophthalic acid (homophthalic acid), homophthalic acid, and homophthalic acid, Phthalic acid (phthalonic acid), isophtalonic acid, terephthalonic acid (terephthalic acid), cumic acid, ursolic acid (uvitic acid), benzoic acid, phthalic acid, salicylic acid, and the like. These may be contained alone or in combination.
Among the salts of the aromatic carboxylic acid compound, ammonium salts, sodium salts, lithium salts, and potassium salts of the aromatic carboxylic acid compound are more preferable, which are excellent in the effect of preventing fusion welding during plastic working (fusion welding resistance).
In addition, in the salt of the aromatic carboxylic acid compound, when a plurality of carboxyl groups are directly bonded to the benzene ring, at least a part of the carboxyl groups may be formed into a salt, or all of the carboxyl groups may be formed into a salt. For example, in the case of a sodium salt of phthalic acid having two carboxyl groups, sodium hydrogen phthalate in which one side carboxyl group is salified with sodium, and disodium phthalate in which both side carboxyl groups are salified with sodium may be contained.
The peroxide of the aromatic carboxylic acid compound is a compound having a peroxide structure on at least one carboxyl group among carboxyl groups directly bonded to the benzene ring of the aromatic carboxylic acid compound. For example, in the case where the aromatic carboxylic acid compound is benzoic acid, the peroxide thereof is peroxybenzoic acid.
In the case where a plurality of carboxyl groups are directly bonded to the benzene ring, at least a part of the peroxide of the aromatic carboxylic acid compound may have a peroxide structure.
The aromatic carboxylic acid compound, a salt thereof, or a peroxide thereof is not necessarily contained in the raw material, and may be contained in the 2 nd film to be formed. For example, an acid anhydride of a carboxylic acid directly bonded to a benzene ring (e.g., phthalic anhydride) is reacted with water or an alcohol to produce a compound having a benzene ring to which a carboxyl group is bonded.
The content of the aromatic carboxylic acid compound in the 2 nd film is not particularly limited, and the 2 nd film may contain a compound other than the aromatic carboxylic acid compound, for example, another resin, within a range not to impair the effects of the present invention. When the compound other than the aromatic carboxylic acid compound is contained in the 2 nd film, the content of the aromatic carboxylic acid compound in the 2 nd film may be 0.5 wt% or more, preferably 10 wt% or more. The 2 nd film may be formed only of an aromatic carboxylic acid compound.
1-4. a coating film included between the 1 st coating film and the 2 nd coating film
The metal material for plastic working may include a single-layer or multi-layer film laminated between the 1 st film and the 2 nd film.
The film included between the 1 st film and the 2 nd film, the type, material, combination of materials, combination of film treatment methods, number of layers, thickness of each film, and the like are not particularly limited as long as the effects of the present invention are not impaired.
The film included between the 1 st film and the 2 nd film may include a chemical film, a coating film, a plating film, an oxide film, or the like. For example, a plating film can be formed on the 1 st film by vapor deposition or other vapor phase plating, and then a chemical film or the like can be further formed on the plating film.
2. Method for producing metal material for plastic working
A method for producing a metal material for plastic working according to another embodiment of the present invention includes: a1 st coating film forming step of forming a1 st coating film on at least a surface of the metal material; and a2 nd film forming step of forming a2 nd film on the surface of the 1 st film.
The step of washing with water may be included before or after each step in the step of forming the 1 st film, or the step of drying may be included after the step of forming the 1 st film. In the 2 nd film forming step, similarly, a water washing step may be included before and after each step, or a drying step may be included after the 2 nd film is formed. Further, when the surface treatment layer is formed between the 1 st film and the 2 nd film, a water washing step may be included between the steps, or a drying step may be included after the film is formed.
If necessary, a step of forming a single layer or a plurality of layers of films may be included after the 1 st film is formed and before the 2 nd film is formed.
Further, before and after each step, a cleaning step may be included. The cleaning step may be performed a plurality of times.
2-1. the 1 st film-forming step
The 1 st film forming step may include at least one of a chemical synthetic film forming step and a coating film forming step.
2-1-1. formation of chemically synthesized leather film
The chemical synthetic leather film forming process at least comprises a contact process: a chemical synthesis treatment agent is brought into contact with the surface of a metal material to form a1 st coating film as a chemical synthesis coating film. The contact method is not particularly limited, and a known method can be used. Examples thereof include: an electrolysis treatment method by applying an electric current, and a treatment method without applying an electric current, such as an immersion treatment method, a spray treatment method, and a spraying treatment method.
The (contact) temperature of the metal material and the chemical synthesis treatment agent is not particularly limited, and examples thereof include: preferably 10 ℃ or higher and 98 ℃ or lower, and more preferably 20 ℃ or higher and 50 ℃ or lower.
The contact time is not particularly limited, but is preferably, for example, 30 to 300 seconds, and more preferably 60 to 180 seconds.
2-1-2. coating film Forming step
The coating film forming step includes at least the following steps: a treatment agent for forming a coating film is brought into contact with the surface of a metal material or on the surface of the metal material to form a1 st coating film as a coating film. The contact method is not particularly limited, and a known method can be used. The coating film can be formed by applying, for example, a roll coating method, a dipping method, a flow coating method, a spraying method, a brush coating method, an electrostatic coating liquid method, a bar coating method, a powder coating method, or the like. More specifically, for example, when the metal material is in the form of a sheet, the roll coating method or the spray coating method is preferably performed. Further, if the metal material is a molded article, it is preferable to carry out the dipping method. In the case where the raw material contains a solid, the solid raw material may be dissolved or dispersed in a solvent such as water or an organic solvent in advance, and then the treatment agent may be prepared.
The amount of the coating film deposited is not particularly limited, but is, for example, 0.5g/m2Above and 50.0g/m2Hereinafter, it is preferably 2.0g/m2Above and 20.0g/m2Hereinafter, more preferably 2.0g/m2Above and 10.0g/m2The following. The amount of the above-mentioned adhesion can be adjusted by changing the composition, concentration, etc. of the treating agent, or by changing the contact conditions such as the contact method, contact temperature, contact time, etc.
The contact conditions of the above-mentioned treating agents are not particularly limited. For example, the temperature of the treatment agent when the treatment agent is contacted is 10 ℃ or more and 80 ℃ or less, preferably 25 ℃ or more and 75 ℃ or less, and more preferably 25 ℃ or more and 60 ℃ or less, but is not limited thereto. The contact time can be set as appropriate, and is usually 2 seconds or more and 180 seconds or less.
The 1 st film forming step may include a drying step as necessary. The drying method is not particularly limited, and a known method can be used. Examples thereof include: natural drying, drying under reduced pressure, convection heating drying (e.g., natural convection heating drying, forced convection heating drying), radiation drying (e.g., near infrared drying, far infrared drying), ultraviolet curing drying, electron beam curing drying, vapor curing (vapor cure), and the like. Further, a plurality of these may be combined and used.
The drying time may be appropriately selected according to the composition of the treating agent. The drying time is preferably in the range of 1 second to 1800 seconds, more preferably 10 seconds to 1200 seconds.
The drying temperature is not particularly limited as long as it is a normal drying temperature, and the metal peak temperature (PMT) of the metal material is preferably 60 ℃ to 150 ℃, and more preferably 80 ℃ to 150 ℃. When the drying temperature is less than 60 ℃, water as a main solvent of the surface treatment agent may remain, and the film may not be fixed on the surface of the metal material. In this case, it is also possible to maintain the temperature at a temperature of less than 60 ℃ until the moisture is volatilized. Since the productivity is lowered by continuing the drying until the moisture is volatilized, the above-mentioned drying temperature of 60 ℃ or more is preferable.
2-2. method for forming coating film included between 1 st coating film and 2 nd coating film
The method for producing the coating film included between the 1 st coating film and the 2 nd coating film includes a coating film forming step: a desired single-layer or multilayer film is formed on the surface of the 1 st film. The coating forming step is not particularly limited, and a known method corresponding to the coating to be formed can be used. Examples thereof include: a chemical synthesis treatment step of forming a chemical synthesis film, a contact step and a drying step of a treatment agent for forming a coating film and a metal material on which the 1 st film is formed, a plating treatment step of forming a plating film, and the like. The processing conditions in each step are not particularly limited, and processing conditions suitable for each coating and the method for forming the coating can be used.
2-3. 2 nd coating film formation step
The 2 nd film forming step includes the steps of: the treating agent for forming the 2 nd film is brought into contact with the surface or the surface of the 1 st film formed on the surface or the surface of the metal material. The contact method is not particularly limited, and any method similar to the contact method in the coating film forming step can be used. In addition, in the case where the raw material contains a solid, the solid raw material may be dissolved or dispersed in a solvent such as water or an organic solvent in advance, and then the treatment agent may be prepared.
The contact conditions of the above-mentioned treating agents are not particularly limited. For example, the temperature of the treatment agent when the treatment agent is contacted is 10 ℃ or more and 80 ℃ or less, preferably 25 ℃ or more and 75 ℃ or less, and more preferably 25 ℃ or more and 60 ℃ or less, but is not limited thereto. The contact time can be set as appropriate, but is usually 2 seconds or more and 180 seconds or less.
The 2 nd film forming step may include a drying step as necessary. The drying method is not limited to the contact method of the coating film, and the same method as the drying method of the coating film can be used.
The drying time can be appropriately selected from the most suitable conditions according to the composition of the treating agent, but is preferably in the range of 1 second to 1800 seconds, more preferably 10 seconds to 1200 seconds, from the viewpoint of productivity and film formation.
The drying temperature is not particularly limited as long as it is a normal drying temperature, and the metal peak temperature (PMT) of the metal material is preferably 60 ℃ to 150 ℃, and more preferably 80 ℃ to 150 ℃. When the drying temperature is 60 ℃ or higher, water as a main solvent of the surface treatment agent is less likely to remain, and the coating film is easily fixed on the surface of the metal material, which is also preferable in terms of corrosion resistance.
The amount of the 2 nd coating deposited is not particularly limited, but is, for example, 0.1g/m2Above and 20.0g/m2Hereinafter, it is preferably 2.0g/m2Above and 15.0g/m2The following. The amount of the deposit can be adjusted by changing the composition, concentration, etc. of the treating agent, or by changing the contact conditions such as the contact method, contact temperature, and contact time.
2-4. cleaning procedure
The cleaning step is a step of cleaning the surfaces of the metal material, the 1 st coating film, and each coating film included between the 1 st coating film and the 2 nd coating film by, for example, water washing (e.g., hot water washing), solvent washing, alkali degreasing washing, acid washing, or the like.
The cleaning step is performed for the purpose of removing oil, dirt, and scale adhering to the surface or surfaces of the metal material, the 1 st film, and each film included between the 1 st film and the 2 nd film during the operation. Further, a rust preventive oil is sometimes applied to the surface or the surface of the metal material for rust prevention, and in this case, the purpose also includes removal of the rust preventive oil. By performing the cleaning step, the surface or the surface can be cleaned, and the surface or a treatment agent for a coating film laminated on the surface can be brought into uniform contact with the surface. Further, when the surface or the surface is free from oil or dirt and the chemical synthesis treatment agent or the coating material can be brought into uniform contact with the surface, the cleaning step is not particularly required.
3. Plastic working method
The plastic working method of the present embodiment is not particularly limited, and examples thereof include known methods such as forging, extrusion, drawing, pipe drawing, crimping, bending, joining, shearing, and shaping.
Examples
Hereinafter, the effects of the present invention will be specifically described by referring to examples of the present invention and comparative examples. In addition, the present invention is not limited to these examples.
(1-1) metallic Material the metallic materials used in examples 1 to 19 and comparative examples 1 to 4 were in the shape of a barrel having a heading rate of 45% based on the ball reducing die press type friction test method disclosed in the reference (Kogaqiao Zhaozhi, guang zaoren, Xiao shann, Shigella wangensis: Jun-Tu proceedings of 62 nd Union of Plastic working (2011), 89-90).
As for the material of the above metal material, S10C material was used in examples 1 to 10 and comparative examples 1, 3 and 4, and SUS430 material was used in examples 11 to 19 and comparative example 2.
(1-2) preparation of various surface-treating agents
Surface treatment agents for forming the 1 st and 2 nd films of examples 1 to 19 were prepared in the combinations shown in table 1. Hereinafter, the surface treatment agent for forming the 1 st film will be referred to as a surface treatment agent a, and the surface treatment agent for forming the 2 nd film will be referred to as a surface treatment agent B.
Surface treating agent A
Surface treating agents A of examples 1 to 10 were prepared. First, Palbond 181XM (manufactured by Karmax Kogyo Co., Ltd.) was added to deionized water so that the concentration became 90.0 g/L. Then, the value of total acidity determined by the titration method was divided by the value of free acidity determined by the same method, and this was regarded as the acid ratio (total acidity/free acidity), and it was confirmed that the acid ratio was 6.5.
Subsequently, the concentration (unit: dot) of the accelerator 131 (manufactured by tradename of rice-flour-paste japan) was adjusted to 2.5 dots.
The concentration of the accelerator 131 was measured using a glass instrument called a saccharimeter (capacity 50 mL). In the concentration measurement, the surface treatment agent to which the accelerator was added was charged into a sugar meter, and 5g of reagent 205 (manufactured by jakeka rice-flour-rice-flour company) that reacted with the accelerator contained in the surface treatment agent was added. At this time, if the surface treatment agent contains an accelerator, gas is generated. The volume of the generated gas represents the concentration of the accelerator, and if the amount of the generated gas is 1mL, the concentration (unit: dot) of the accelerator contained in the surface treatment agent is 1 dot.
Surface-treating agents A of examples 11 to 19 were prepared. First, Felbond A1 and Felbond A2 (both manufactured by Karmax Kogyo Co., Ltd.) were added to deionized water so that the former concentration was 40.0g/L and the latter concentration was 20.0 g/L. Next, the concentration of the accelerator using the accelerator 16 (manufactured by japan tradename, etc.) was adjusted to 1.0 point.
The concentration of accelerator 16 was titrated as follows: the surface-treated liquid was collected in a beaker with a 25mL whole pipette, and 50mL of deionized water, 25.0mL of reagent 54 (manufactured by jascara rice-flour noodles), and indicator 10 (manufactured by jascara rice-flour noodles) were added, and titration was performed with titrant 53 (manufactured by jascara rice-flour noodles) until the liquid became deep blue. The required dropping amount of the titration liquid 53 is defined as the accelerator concentration (unit: dot).
Surface treatment agent B
The surface treatment agent B was prepared by adding the aromatic carboxylic acid compound described in table 1, a salt thereof, or a peroxide thereof to distilled water. The concentration of the aromatic carboxylic acid compound, the salt thereof, or the peroxide thereof in the surface-treating agent B was controlled so that the amount of the 2 nd film formed from the surface-treating agent B adhered was 4.0g/m2、8.0g/m2、12g/m2。
The following surface treatment agents were used as the surface treatment agents for forming a single coating film in comparative examples 1 to 4.
Surface treatment agent in comparative example 1: the surface treating agent A of examples 1 to 10.
Surface treatment agent in comparative example 2: the surface treating agent A according to examples 11 to 19.
Surface treatment agent in comparative example 3: mineral oil (paraffin mineral oil 8cst (centistokes) at 40 ℃).
Surface treatment agent in comparative example 4: surface treating agent B of examples 2 and 12
(1-3) cleaning treatment of metallic Material
The surfaces of the metal materials used in the above examples and comparative examples were cleaned by the following methods.
The concentration of a commercially available degreaser (Fine Cleaner E6400, tradename of JAPONICA) was adjusted to 20g/L using tap water, and the mixture was heated to 60 ℃ and maintained at a constant temperature. The metal material was immersed in the degreasing agent for 10 minutes to degrease. Subsequently, the degreaser, dirt, and the like remaining after 20 seconds of immersion in 25 ℃ tap water were washed off with water. Subsequently, the metal material after washing was immersed in 17.5% hydrochloric acid at 25 ℃ for 10 minutes to remove the dirt which could not be removed by washing. Further, the metal material was immersed in tap water at 25 ℃ for 20 seconds, and hydrochloric acid adhering to the metal material was washed off.
(1-4) method for forming the No. 1 film and the No. 2 film of examples 1 to 19
The metal material subjected to the cleaning treatment was formed into the 1 st film and the 2 nd film by the following method.
Examples 1 to 10
The cleaned metal material was immersed in the surface treatment agent a adjusted to 80 ℃ for 10 minutes to form a1 st film. Subsequently, the metal material on which the 1 st coating was formed was immersed in tap water at 25 ℃ for 30 seconds and washed with water. Table 1 shows the amount of the first film deposited in examples 1 to 10. The adhesion amount was calculated by measuring the weight of the metal material before and after formation of the 1 st coating, determining the difference as the adhesion weight, and dividing by the original surface area of the metal material.
Further, the metal material on which the 1 st film was formed was immersed in the surface treatment agent B heated to 60 ℃ for 15 seconds, and after taking out, it was naturally dried to form a2 nd film as the metal material for plastic working of examples 1 to 10. Table 1 shows the amount of the coating deposited on the 2 nd coating. The adhesion amount was calculated by measuring the weight of the metal material before and after the formation of the 2 nd coating, and dividing the difference by the surface area of the original metal material to obtain the adhesion weight.
Examples 11 to 19
The cleaned metal material was immersed in the surface treatment agent a adjusted to 90 ℃ for 10 minutes to form a1 st film. Subsequently, the metal material on which the 1 st coating was formed was immersed in tap water at 25 ℃ for 30 seconds, and washed with water. Table 1 shows the amount of the first coating film deposited in examples 11 to 19. The amount of adhesion was calculated by the same method as in examples 1 to 10.
Further, the metal material on which the 1 st film was formed was immersed in the surface treatment agent B heated to 60 ℃ for 15 seconds, and after taking out, it was naturally dried to form a2 nd film as the metal material for plastic working of examples 11 to 19. Table 1 shows the amount of the coating deposited on the No. 2 coating films of examples 11 to 19. The amount of adhesion was calculated by the same method as in examples 1 to 10.
(1-5) method for Forming Single coating film of comparative examples 1 to 4
In comparative example 1, a single film was formed by the same method as the method for forming the first film in examples 1 to 10, and then the metal material was immersed in tap water at 25 ℃ for 30 seconds and washed with water to obtain a metal material for plastic working in comparative example 1.
In comparative example 2, a single film was formed by the same method as that for the first film in examples 11 to 19, and then the metal material was immersed in tap water at 25 ℃ for 30 seconds and washed with water to obtain a metal material for plastic working in comparative example 2.
In comparative example 3, the substrate was immersed in mineral oil heated to 40 ℃ for 10 seconds, then taken out, and excess mineral oil was wiped off to increase the amount of adhesion (g/m) of the mineral oil2) Becomes 4.0g/m2The metal material for plastic working of comparative example 3 was prepared.
In comparative example 4, a single film was formed by the same method as the method for forming the 2 nd film in examples 2 and 12, and then the metal material was immersed in tap water at 25 ℃ for 30 seconds and washed with water to obtain a metal material for plastic working of comparative example 4.
Table 1 shows the amount of the single film deposited in comparative examples 1 to 4.
(1-6) evaluation test
(1-6-1) ball reducing squeeze test
Evaluation of fusion resistance and lubricity was performed based on the ball reducing squeeze friction test method disclosed in the above reference.
The evaluation test was carried out as follows: after the film was formed, the side portions protruding from the barrel test piece were subjected to reducing extrusion (hard working) using 3 spherical dies (SUJ-2 bearing balls having a diameter of 10 mm). The evaluation of the fusion-weld resistance of each test piece was judged by visually observing the appearance of the latter half of the reducing extrusion in which the surface area was enlarged, based on the evaluation criterion (a shown in fig. 1 is the optimum one). The lubricity of each test piece was evaluated according to the following evaluation criteria.
In addition, in the present embodiment, there is no difference in corrosion resistance (comparison of rust conditions under equivalent environments) before and after plastic working, and therefore, it can be considered that: the 2 nd film remains after plastic working, and the 1 st film is protected.
< evaluation criteria for lubricity >
The lubricity was evaluated by comparing the maximum load value obtained at the time of the reducing extrusion processing with the range of the maximum load value as an evaluation criterion described below. The smaller the maximum load value, the more excellent the lubricity.
A: the maximum load value is less than 38 kN.
B: the maximum load value is 38kN or more and less than 40 kN.
C: the maximum load value is 40kN or more and less than 42 kN.
D: the maximum load value is 42kN or more.
[ Table 1]
TABLE 1
Figure BDA0002638155630000151
[ Table 2]
TABLE 2
Resistance to fusion welding Lubricity of
Example 1 A A
Example 2 A A
Example 3 A A
Example 4 A A
Example 5 A A
Example 6 A A
Example 7 A A
Example 8 A A
Example 9 A B
Example 10 A A
Example 11 A A
Example 12 A A
Example 13 A A
Example 14 A A
Example 15 B A
Example 16 A B
Example 17 A A
Example 18 B A
Example 19 A A
Resistance to fusion welding Lubricity of
Comparative example 1 E D
Comparative example 2 E D
Comparative example 3 E D
Comparative example 4 D C
It should be noted that although the present invention has been described in detail with reference to specific examples, it is apparent to those skilled in the art that various changes and modifications can be made without departing from the spirit and scope of the present invention.

Claims (1)

1. A metal material for plastic working, which comprises a1 st film on the surface of the metal material and a2 nd film on the surface of the 1 st film,
the No. 2 skin film is a surface layer,
the 2 nd film contains a peroxide of a compound having a benzene ring directly bonded to at least 1 carboxyl group, a salt of a compound having a benzene ring directly bonded to at least 1 carboxyl group, or a compound having a benzene ring directly bonded to at least 1 carboxyl group.
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