Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
  • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES, PROFILES OR LIKE SEMI-MANUFACTURED PRODUCTS OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
  • B21C23/00—Extruding metal; Impact extrusion
  • B21C23/32—Lubrication of metal being extruded or of dies, or the like, e.g. physical state of lubricant, location where lubricant is applied
• • 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
  • C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or 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
  • C23C22/05—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
  • C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
  • C23C22/56—Treatment of aluminium or alloys based thereon
• • 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

Definitions

• the present invention relates to a metal surface pretreatment agent.
• the lubricant for example, liquid lubricants such as mineral oil, synthetic oil, and vegetable oil have been used for a long time.
• these lubricants can be applied to relatively simple plastic working, their lubricating performance is insufficient in plastic working in which they slide under high surface pressure and generate a large amount of heat.
• a lubricating film chemical conversion treatment is performed on the material surface (
• the method of performing aluminum fluoride zinc fluoride treatment is widely adopted. Specifically, an aqueous solution of zinc fluoride (ZnF 2 ) and sodium silica fluoride is used to form a film of aluminum fluoride and zinc fluoride on the aluminum surface, and a film of this zinc compound and soap as a lubricant. Surface lubricity is ensured by making (metal soap).
• Patent Document 1 discloses a method of forming a clayified film (layered double hydroxide) on an aluminum surface using an aqueous solution of a zinc compound.
• This clayified film is a clay substance having a layered structure containing zinc hydroxide and aluminum hydroxide as main components, and is formed by a simple process of simply immersing aluminum in an aqueous zinc solution.
• the method for synthesizing the clayified film (claying method) disclosed in Patent Document 1 can be replaced with the current existing method of aluminum-zinc fluoride treatment.
• the clayified film contains zinc hydroxide having a strong bond with soap which is a lubricant, a lubricating film can be formed on the aluminum surface.
• this clayification method has an advantage that the treatment liquid does not need to be frequently renewed because aluminum does not accumulate in the coating treatment liquid unlike the aluminum fluoride zinc treatment method. Furthermore, it has the advantage that it is not necessary to use fluorine, which is a harmful substance, unlike the above-mentioned aluminum fluoride zinc fluoride treatment.
• the reaction time of the clayification method of Patent Document 1 requires 24 hours or more, there remains a problem in practical use. Further, the clayified film formed by the clayification method of Patent Document 1 and the lubricant (soap) form a composite film, and it is also required to further enhance the lubricity of the composite film.
• the present invention can rapidly form a film containing zinc on the surface of a metal material, and further, by applying a lubricant to the film, excellent lubricity is exhibited.
• the main purpose is to provide a pretreatment agent for metal surfaces.
• Another object of the present invention is to provide a metal surface treatment kit, a metal processing kit, a metal surface treatment method, and a metal processing method using the metal surface pretreatment agent.
• an aqueous liquid containing an alkaline component containing at least one of calcium, potassium and sodium is used as a metal surface pretreatment agent to pretreat the surface of the metal material, and after the pretreatment, a zinc compound is contained.
• a film containing zinc is rapidly formed on the surface of the metal material, and further, by applying a lubricant to the film, plastic processing of the metal material is performed. It was found that the surface of the metal material exhibits excellent lubricity.
• the present invention is an invention completed by further studying based on these findings.
• Item 1 A pretreatment agent used before a treatment in which a film-forming treatment agent containing a zinc compound is brought into contact with the surface of a metal material to form a film containing zinc.
• the pretreatment agent is a metal surface pretreatment agent which is an aqueous liquid containing an alkaline component containing at least one of calcium, potassium and sodium.
• Item 2. The metal surface pretreatment agent according to Item 1, wherein the film does not contain a fluorine atom.
• Item 3. Item 2. The metal surface pretreatment agent according to Item 1 or 2, wherein the metal surface pretreatment agent contains at least one of calcium hydroxide, potassium hydroxide and sodium hydroxide as the alkaline component.
• Item 2. The metal surface pretreatment agent according to any one of Items 1 to 3, wherein the concentration of the alkaline component is 0.01 to 10 mol / L.
• Item 5. Item 2. The metal surface pretreatment according to any one of Items 1 to 4, wherein the surface of the metal material is composed of aluminum, zinc, magnesium, iron, copper, or an alloy containing at least one of these metals. Agent.
• Item 6. The first agent comprising the metal surface pretreatment agent according to any one of Items 1 to 5 and A second agent consisting of a film-forming treatment agent containing a zinc compound, A kit for metal surface treatment.
• Item 7. Item 6.
• the first agent comprising the metal surface pretreatment agent according to any one of Items 1 to 5 and A second agent consisting of a film-forming treatment agent containing a zinc compound, A third agent consisting of a lubricant and A kit for metal processing.
• a metal surface treatment method comprising a pretreatment step of bringing the metal surface pretreatment agent according to any one of Items 1 to 5 into contact with the surface of a metal material.
• a film forming step of bringing a film forming treatment agent containing a zinc compound into contact with the surface of the metal material to which the metal surface pretreatment agent is attached is provided.
• Film formation treatment method is provided.
• the pretreatment step of bringing the metal surface pretreatment agent according to any one of Items 1 to 5 into contact with the surface of the metal material and After the pretreatment step, a film forming step of bringing a film forming treatment agent containing a zinc compound into contact with the surface of the metal material which has been brought into contact with the metal surface pretreatment agent.
• a zinc-containing film can be rapidly formed on the surface of the metal material after the pretreatment, and the film can be lubricated.
• the agent it is possible to provide a metal surface pretreatment agent that exhibits excellent lubricity.
• the metal surface pretreatment agent of the present invention is used before the treatment of contacting (adhering) a film-forming treatment agent containing a zinc compound to form a zinc-containing film on the surface of a metal material.
• the agent is an aqueous liquid containing an alkaline component containing at least one of calcium, potassium and sodium. Since the metal surface pretreatment agent of the present invention has this structure, a zinc-containing film is formed by contacting (adhering) a film-forming treatment agent containing a zinc compound to the surface of the metal material after pretreatment. Is formed quickly, and by applying a lubricant to the film, the surface of the metal material exhibits excellent lubricity in the plastic processing of the metal material. A metal material with improved lubricity has excellent plastic workability.
• the metal surface pretreatment agent of the present invention will be described in detail.
• the aqueous liquid containing an alkaline component containing at least one of calcium, potassium and sodium is specifically an alkaline component containing at least one of calcium, potassium and sodium.
• the contained aqueous suspension or aqueous solution may be in the form of an aqueous suspension or an aqueous solution.
• the metal surface pretreatment agent of the present invention is preferably an aqueous suspension.
• the metal surface pretreatment agent of the present invention is preferably an aqueous suspension.
• the metal surface pretreatment agent of the present invention is preferably an aqueous suspension.
• the metal surface pretreatment agent of the present invention is a pretreatment agent that is subjected to surface treatment of a metal material by contacting (adhering) to the surface of the metal material.
• a metal material surface-treated with the metal surface pretreatment agent of the present invention is brought into contact (adhesion) with a film-forming treatment agent containing a zinc compound, a zinc-containing film is preferably formed. That is, at least one of calcium, potassium and sodium contained in the metal surface pretreatment agent adhering to the metal surface is rapidly replaced with zinc contained in the film forming treatment agent, and a film containing zinc on the surface of the metal material. Is preferably formed. Then, the metal material having a zinc-containing film formed on its surface can be suitably subjected to plastic working by applying a lubricant.
• the metal surface pretreatment agent of the present invention is an aqueous liquid containing an alkaline component containing at least one of calcium, potassium and sodium.
• an alkaline component calcium hydroxide (Ca (OH) 2 ), potassium hydroxide (KOH), sodium hydroxide (NaOH) and the like are preferable, and calcium hydroxide (Ca (OH) 2 ) is particularly preferable.
• the metal surface pretreatment agent of the present invention is preferably at least one of a calcium hydroxide aqueous liquid, potassium hydroxide and sodium hydroxide aqueous liquid, and is particularly preferably a calcium hydroxide aqueous liquid.
• the calcium hydroxide aqueous liquid is particularly preferably a calcium hydroxide aqueous suspension.
• the concentration of the alkaline component is not particularly limited, but is preferably 0.01 to 0.01 from the viewpoint of forming a zinc-containing film on the surface of the metal material after the pretreatment particularly quickly. It is about 10 mol / L, more preferably about 0.03 to 5 mol / L, and even more preferably about 0.05 to 1 mol / L.
• the temperature at which the metal surface pretreatment agent of the present invention is brought into contact (adhesion) with the surface of the metal material to pretreat the metal surface is not particularly limited, but the surface of the metal material after the pretreatment is coated with a zinc-containing film. Is preferably about 20 to 90 ° C., more preferably about 30 to 80 ° C., still more preferably about 40 to 80 ° C., and particularly preferably about 60 to 80 ° C. from the viewpoint of forming the above quickly.
• the time for contacting the metal surface pretreatment agent of the present invention with the surface of the metal material is not particularly limited, but is preferable from the viewpoint of forming a zinc-containing film on the surface of the metal material after the pretreatment particularly quickly. It is 1 hour or less, more preferably 30 minutes or less, still more preferably 20 minutes or less, and particularly preferably 10 minutes or less.
• the lower limit of the time for the metal surface pretreatment agent of the present invention to come into contact with the surface of the metal material is preferably 30 seconds or longer, more preferably 1 minute or longer.
• the method of contacting (adhering) the metal surface pretreatment agent of the present invention to the surface of the metal material is not particularly limited, and is carried out by a known method such as a roll coating method, a spin coating method, a spray method, or a dipping method. be able to.
• the main purpose of cleaning the surface of a metal material is to remove various stains (oil, etc.) adhering to the surface of the metal material.
• the method for cleaning the surface of the metal material is not particularly limited, and for example, a method using a known cleaning agent such as an alkaline degreasing agent or an acidic degreasing agent can be adopted. Further, in the washing, it is preferable to wash with water.
• the treatment agent for forming a film containing a zinc compound is not particularly limited as long as it comes into contact with (adheres) to the surface of the metal material to form a film containing zinc, and is used for plastic working of metal materials and the like.
• a known film-forming treatment agent can be used.
• the zinc compound is not particularly limited as long as it is water-soluble, but zinc nitrate, zinc sulfate, zinc chloride and the like are preferable, and zinc nitrate is particularly preferable.
• the zinc compound contained in the film-forming treatment agent may be one kind or two or more kinds.
• the film containing zinc is, for example, a clay substance having a layered structure containing zinc hydroxide and aluminum hydroxide as main components (clay of layered double hydroxide) as described in Patent Document 1. A layer formed by a film) can be mentioned.
• the film-forming treatment agent containing a zinc compound examples include an aqueous solution of zinc nitrate, an aqueous solution of zinc sulfate, an aqueous solution of zinc chloride, and the like, and an aqueous solution of zinc nitrate is particularly preferable.
• the zinc-containing film formed on the metal material preferably does not contain fluorine atoms. That is, it is preferable that the film-forming treatment agent containing a zinc compound does not contain a component containing a fluorine atom.
• the concentration of the zinc compound is not particularly limited, but zinc is brought into contact (adhesion) with the surface of the metal material surface-treated with the metal surface pretreatment agent of the present invention. From the viewpoint of forming the containing film particularly rapidly, it is preferably about 0.05 to 10 mol / L, more preferably about 0.08 to 5 mol / L, and further preferably about 0.1 to 1 mol / L.
• the pH of the film-forming treatment agent containing a zinc compound is not particularly limited, but the zinc-containing film can be formed by contacting (adhering) with the surface of the metal material surface-treated with the metal surface pretreatment agent of the present invention.
• it is preferably about 5 to 7, and more preferably about 5.5 to 6.5.
• ammonia water or the like may be added to the film-forming treatment agent.
• a temperature at which a film-forming treatment agent containing a zinc compound is brought into contact (adhesion) with the surface of a metal material surface-treated with the metal surface pretreatment agent of the present invention to form a zinc film on the metal surface Is not particularly limited, but is preferably 30 to 100 from the viewpoint of forming a zinc-containing film particularly quickly by contacting (adhering) with the surface of the metal material surface-treated with the metal surface pretreatment agent of the present invention.
• the temperature is about ° C., more preferably about 40 to 90 ° C., further preferably about 60 to 85 ° C., and particularly preferably about 65 to 85 ° C.
• the time for contacting the film-forming treatment agent containing the zinc compound with the surface of the metal material surface-treated with the metal surface pretreatment agent of the present invention is not particularly limited, but the surface treatment with the metal surface pretreatment agent of the present invention is not particularly limited. From the viewpoint of forming a zinc-containing film particularly quickly by contacting with the surface of the metal material, preferably 1 hour or less, more preferably 30 minutes or less, still more preferably 20 minutes or less, particularly preferably 10 minutes or less. Is.
• the lower limit of the time for the metal surface pretreatment agent of the present invention to come into contact with the surface of the metal material is preferably 30 seconds or longer, more preferably 1 minute or longer.
• the method of contacting (adhering) the film-forming treatment agent containing the zinc compound to the surface of the metal material surface-treated with the metal surface pretreatment agent of the present invention is not particularly limited, and is, for example, a roll coating method or a spin. It can be carried out by a known method such as a coating method, a spray method, or a dipping method.
• the metal constituting the metal material preferably contains aluminum, zinc, magnesium, iron, copper, or at least one of these metals.
• examples thereof include alloys, and aluminum is particularly preferable.
• the surface of the metal material to be treated by the metal surface pretreatment agent of the present invention is preferably composed of aluminum, zinc, magnesium, iron, copper, or an alloy containing at least one of these metals. , It is particularly preferable that it is composed of aluminum.
• the metal material on which the zinc-containing film is formed can be subjected to plastic working after being lubricated.
• a known lubrication treatment method which is performed in plastic working of a metal material, can be adopted.
• the lubricant component of the lubricant those lubricated with a solid lubricant such as molybdenum disulfide or graphite, or those lubricated with oil, soap, etc. are widely used.
• Soap is preferably used as a lubricant because it binds to zinc to form a metal soap, so that it is strongly bonded, and the viscosity decreases due to heat generation during plastic processing to improve lubricity.
• soaps and oils that do not bind to zinc are also effective for lubricity. Only one type of lubricant component may be used, or two or more types may be mixed and used.
• Oils include saturated fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid and lignoceric acid, palmitoleic acid, oleic acid, elaidic acid, linoleic acid, linolenic acid, arachidonic acid and eikosapentaenoic acid. , Unsaturated fatty acids such as docosahexaenoic acid, and fatty acids having about 12 to 26 carbon atoms such as branched fatty acids.
• fatty acids having about 12 to 26 carbon atoms saturated fatty acids such as lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid, behenic acid, lignoseric acid, palmitreic acid, oleic acid, ellagic acid, linole).
• metal soap obtained by reacting with at least one metal selected from zinc, calcium, barium, aluminum, and magnesium.
• the lubricant can be used in the form of an aqueous solution of the above-mentioned lubricant component.
• concentration of the lubricant component in the aqueous solution is not particularly limited as long as a predetermined amount of the lubricant component adheres to the metal material, and examples thereof include about 0.5 to 10% by mass.
• the temperature in the lubrication treatment is not particularly limited, and known lubrication treatment conditions for the surface of the metal material can be adopted, for example, about 30 to 100 ° C., preferably about 40 to 90 ° C., and more preferably 60 to 60 to. It is about 90 ° C.
• the metal surface treatment kit of the present invention comprises a first agent composed of the above-mentioned metal surface pretreatment agent of the present invention and a second agent composed of the above-mentioned film-forming treatment agent containing a zinc compound. It is characterized by being prepared.
• the surface of the metal material is pretreated with the first agent composed of the above-mentioned metal surface pretreatment agent of the present invention, and subsequently, the first agent composed of a film forming treatment agent containing a zinc compound.
• the first agent composed of a film forming treatment agent containing a zinc compound.
• metal surface pretreatment agent of the present invention Details of the metal surface pretreatment agent of the present invention, the film-forming treatment agent containing a zinc compound, and the lubricant are as described above.
• the metal materials are also as described in the column of "1. Metal surface treatment agent”.
• the metal processing kit of the present invention comprises a first agent composed of the above-mentioned metal surface pretreatment agent of the present invention, a second agent composed of the above-mentioned film-forming treatment agent containing a zinc compound, and a lubricant. It is provided with a third agent comprising.
• the surface of the metal material is pretreated with the first agent composed of the above-mentioned metal surface pretreatment agent of the present invention, and subsequently, the second agent composed of a film forming treatment agent containing a zinc compound is used.
• the surface of the metal material exhibits excellent lubricity in the plastic processing of the metal material.
• a metal material with improved lubricity has excellent plastic workability.
• metal surface pretreatment agent of the present invention Details of the metal surface pretreatment agent of the present invention, the film-forming treatment agent containing a zinc compound, and the lubricant are as described above.
• the metal materials are also as described in the column of "1. Metal surface treatment agent”.
• the metal surface treatment method of the present invention includes a pretreatment step of bringing the above-mentioned metal surface pretreatment agent of the present invention into contact (adhesion) with the surface of a metal material.
• the metal material surface-treated with the metal surface pretreatment agent of the present invention preferably forms a zinc-containing film when a film-forming treatment agent containing a zinc compound is brought into contact (adhesion) with the surface. Will be done. Then, the metal material having a zinc-containing film formed on its surface can be suitably subjected to plastic working by applying a lubricant.
• metal surface treatment agent of the present invention Details of the metal surface treatment agent of the present invention are as described in the column of "1. Metal surface treatment agent”. In addition, the temperature, time, method, etc. when the metal surface pretreatment agent of the present invention is brought into contact (adhesion) with the surface of the metal material to pretreat the metal surface are also described in the column of "1. Metal surface treatment agent”. As described. The metal materials are also as described in the column of "1. Metal surface treatment agent".
• the metal material surface-treated with the metal surface pretreatment agent of the present invention preferably forms a zinc-containing film when a film-forming treatment agent containing a zinc compound is brought into contact (adhesion) with the surface. Will be done. Then, the metal material having a zinc-containing film formed on its surface can be suitably subjected to plastic working by applying a lubricant.
• metal surface pretreatment agent Details of the metal surface pretreatment agent and the film forming treatment agent of the present invention are as described in the column of "1. Metal surface treatment agent”. Further, the temperature, time, method, etc. when the metal surface pretreatment agent of the present invention is brought into contact with the surface of the metal material to pretreat the metal surface are also as described in the column of "1. Metal surface treatment agent”. Is. Further, regarding the temperature, time, method, etc. when the film-forming treatment agent containing a zinc compound is brought into contact with the surface of the metal material to which the metal surface pretreatment agent of the present invention is brought into contact, "1. Metal surface treatment agent”. As described in the column of. The metal materials are also as described in the column of "1. Metal surface treatment agent”.
• a lubricant is applied to the surface of the metal material in which the zinc-containing film is formed by the film forming step of contacting (adhering) the film-forming treatment agent containing the zinc compound to the surface of the (adhered) metal material and the film forming step. It is provided with a lubrication treatment step of bringing the metal material into contact with each other and a metal processing step of subjecting the metal material to plastic processing after the lubrication treatment step.
• the metal material surface-treated with the metal surface pretreatment agent of the present invention preferably forms a zinc-containing film when a film-forming treatment agent containing a zinc compound is brought into contact (adhesion) with the surface. Will be done. Then, the metal material having a zinc-containing film formed on its surface can be suitably subjected to plastic working by applying a lubricant.
• metal surface pretreatment agent Details of the metal surface pretreatment agent, film forming treatment agent and lubricant of the present invention are as described in the column of "1. Metal surface treatment agent”. Further, the temperature, time, method, etc. when the metal surface pretreatment agent of the present invention is brought into contact with the surface of the metal material to pretreat the metal surface are also as described in the column of "1. Metal surface treatment agent”. Is. Further, regarding the temperature, time, method, etc. when the film-forming treatment agent containing a zinc compound is brought into contact with the surface of the metal material to which the metal surface pretreatment agent of the present invention is brought into contact, "1. Metal surface treatment agent”. As described in the column of. Further, the temperature, time, method, etc. when the lubricant is brought into contact with the surface of the metal material on which the zinc-containing film is formed are also as described in the column of "1. Metal surface treatment agent”. The metal materials are also as described in the column of "1. Metal surface treatment agent”.
• Examples 1 to 14 and Comparative Example 2 1.
• a metal surface pretreatment agent, a film-forming treatment agent, and a lubricant were prepared as follows. As will be described later, in Comparative Example 1, the surface treatment of the metal material was performed using a 3% aqueous solution of "Ferorube No. 1" manufactured by Kiwa Chemicals.
• Aluminum material (A5052 material (ring), A5056 material (cylinder), A6061 material (cylinder), respectively, which were used in the tests described later) was mixed with a 3% aqueous solution of "alkylene F700K", a degreasing agent manufactured by Kiwa Chemicals. Treated with water and washed with water. Next, it was immersed in a chemical polishing liquid to adjust the state of the metal surface and washed with water. Next, the aluminum material was immersed in each metal surface pretreatment agent shown in Table 1 at 70 ° C. for 6 minutes and then washed with water.
• each aluminum material was immersed in each film formation treatment solution at the temperature and time shown in the column of "Film formation treatment solution” in Table 1 and adhered in the pretreatment step.
• a film containing zinc hydroxide (a layered double hydroxide clay film) was formed on the surface of the aluminum material by an ion exchange reaction with an alkaline component.
• Comparative Example 1 In Comparative Example 1, a coating film of a metal surface pretreatment agent was formed on the surface of an aluminum material by an aluminum-zinc fluoride treatment method, and lubrication treatment was performed using a 3% aqueous solution of "Ferorube No. 1" manufactured by Kiwa Chemicals. Then, the lubricating film was dried at room temperature to obtain an aluminum material to which the lubricant was attached.
• ⁇ Ring compression test> The material of the ring used in the ring compression test was aluminum A5052, which had an outer diameter of 21.0 mm, an inner diameter of 10.5 mm, and a thickness of 7.0 mm.
• each ring made of an aluminum material to which a lubricant was attached was pressed with a load of 200 tons and a compression ratio of 60%.
• the thickness and inner diameter of the ring after compression were measured, and the coefficient of friction was measured.
• the ring compression test was performed three times each to determine the average friction coefficient ⁇ . In the ring compression test, the relationship between the shape of the ring after compression when it is compressed and the coefficient of friction is known.
• both the inner and outer diameters are compressed so as to project outward.
• the coefficient of friction is large, the inner diameter overhangs inward and the outer diameter also overhangs outward. Therefore, it is possible to measure the dimensional change of the inner diameter portion and calculate the friction coefficient. The lower the coefficient of friction, the higher the lubrication performance.
• the material of the cylindrical test piece used for the implantation test was aluminum A5056, which had a diameter of 40.0 mm and a height of 52.0 mm.
• each cylindrical test piece made of an aluminum material to which a lubricant was attached was pressed under a load of 200 tons and a compression ratio of 30%. After compression, the amount of peeling of the lubricant adhering to the test piece was measured. The implantation test was performed three times each to determine the average peeling amount. The amount of lubricant adhered to the test piece before and after compression can be measured, and the amount of lubricant peeled off can be calculated from the difference in the amount of lubricant adhered to the test piece before and after compression.
• the material of the cylindrical test piece used in the rear extrusion test was aluminum A5056 material and aluminum A6061 material, each of which had a diameter of 29.9 mm and a height of 24.0 mm.
• the rear extrusion friction test is as follows. First, each cylindrical test piece made of an aluminum material to which a lubricant was attached in Examples and Comparative Examples was inserted into a die, and pressed with a load of 200 tons and a compression rate of 20%. The appearance of the test piece after backward extrusion was observed and evaluated according to the following criteria. ⁇ : No seizure ⁇ : Seizure

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