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WO2017038573A1 - Matériau d'alliage d'aluminium, corps lié, élément d'automobile, procédé pour produire un matériau d'alliage d'aluminium, et procédé pour produire un corps lié - Google Patents

Matériau d'alliage d'aluminium, corps lié, élément d'automobile, procédé pour produire un matériau d'alliage d'aluminium, et procédé pour produire un corps lié Download PDF

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Publication number
WO2017038573A1
WO2017038573A1 PCT/JP2016/074628 JP2016074628W WO2017038573A1 WO 2017038573 A1 WO2017038573 A1 WO 2017038573A1 JP 2016074628 W JP2016074628 W JP 2016074628W WO 2017038573 A1 WO2017038573 A1 WO 2017038573A1
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Prior art keywords
film
aluminum alloy
alloy material
resin
precoat layer
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Ceased
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PCT/JP2016/074628
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English (en)
Japanese (ja)
Inventor
明彦 巽
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Kobe Steel Ltd
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Kobe Steel Ltd
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Priority claimed from JP2016035807A external-priority patent/JP2017048456A/ja
Application filed by Kobe Steel Ltd filed Critical Kobe Steel Ltd
Publication of WO2017038573A1 publication Critical patent/WO2017038573A1/fr
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    • 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
    • B32B15/08—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 of synthetic resin
    • 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
    • C23C28/04—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 only coatings of inorganic non-metallic material
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/05—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys of the Al-Si-Mg type, i.e. containing silicon and magnesium in approximately equal proportions

Definitions

  • the present invention relates to an aluminum alloy material, a joined body of the aluminum alloy material and a resin material, an automobile member, a method for producing the aluminum alloy material, and a method for producing the joined body.
  • the method (1) requires bolts, screws, and the like, and is expensive to manufacture. Even in the method (2), it is necessary to separately perform the molding step and the joining step of the resin material. In the method (3), since a through hole is required to be processed, a manufacturing cost is required. In addition, since point bonding is performed, stress concentration is more likely to occur than in the case of surface bonding, and the resistance to fracture and rigidity are structurally disadvantageous. Further, since the method (4) takes time to process, there are problems in terms of productivity and cost when processing large areas and large parts.
  • the present invention provides an aluminum alloy material that is excellent in productivity when manufacturing a bonded body and has high bonding strength and is difficult to reduce the bonding strength, a bonded body of the aluminum alloy material and a resin material, and an automotive member.
  • An object of the present invention is to provide a method for producing the aluminum alloy material and a method for producing the joined body.
  • the present inventors have examined the bonding state between the substrate surface and the adhesive resin layer. And when forming the 1st membrane
  • the present invention is formed on an aluminum alloy substrate and at least a part of the surface of the aluminum alloy substrate, Mg is 0.1 atomic% or more and less than 20 atomic%, Si is 5 atomic% or more and 60 atomic% or less. And a first film made of an oxide film containing less than 0.6 atomic percent of Cu, and a second film having a siloxane bond formed on at least a part of the first film, on a surface 1 of film and the second film is formed, in a spectrum obtained by incidence of parallel polarized light of the incident angle 75 ° by a Fourier transform type infrared spectroscopy, near 1400 cm -1 from 1100 cm -1 An aluminum alloy material having a peak height of 0.01 to 0.50 is provided.
  • an adhesive precoat layer containing a thermoplastic resin may be formed on at least a part of a portion where the first film and the second film are formed.
  • the adhesive precoat layer may have a thickness of 1 to 100 ⁇ m.
  • the present invention also provides a joined body in which the aluminum alloy material is joined to a resin material via the adhesive precoat layer.
  • the thickness of the adhesive precoat layer may be 1 to 100 ⁇ m.
  • the resin forming the resin material may include a thermoplastic resin.
  • the present invention also provides a member for an automobile using the joined body.
  • the present invention provides that at least part of the surface of the aluminum alloy substrate has Mg at least 0.1 atomic% and less than 20 atomic%, Si at 5 atomic% and 60 atomic%, and Cu at 0.6 atomic%.
  • the method for producing an aluminum alloy material comprising: the second film forming step, applying a solution containing a silane coupling agent prepared and allowed to stand for 5 minutes or more to at least a part of the first film;
  • a method for producing an aluminum alloy material which comprises drying at a temperature of 70 ° C. or more within 10 minutes after the application of.
  • the method for producing an aluminum alloy material includes: an adhesive precoat that forms an adhesive precoat layer containing a thermoplastic resin on at least part of a portion of the aluminum alloy material where the first film and the second film are formed.
  • a layer forming step may be further provided.
  • the adhesive precoat layer may have a thickness of 1 to 100 ⁇ m.
  • the present invention also provides a method for manufacturing a joined body, which includes a joining step in which the aluminum alloy material produced by the method for producing an aluminum alloy material is joined to a resin material via the adhesive precoat layer.
  • the adhesive precoat layer may have a thickness of 1 to 100 ⁇ m.
  • the resin forming the resin material may include a thermoplastic resin.
  • the joining step and molding of the resin forming the resin material may be performed simultaneously.
  • the manufacturing method of the joined body may further include a heat treatment step of performing a heat treatment at 80 ° C. or more for 3 minutes or more after the joining step.
  • a heat treatment step of performing a heat treatment at 80 ° C. or more for 3 minutes or more after the joining step you may perform combining the heat processing for 3 minutes or more at 80 degreeC or more, and the cooling process for 3 minutes or more at the temperature below freezing point.
  • the present invention it is possible to realize an aluminum alloy material that is excellent in productivity when manufacturing a bonded body and has high bonding strength and is difficult to decrease in bonding strength.
  • FIG. 1 is a cross-sectional view schematically showing a configuration of an aluminum alloy material according to the first embodiment of the present invention.
  • FIG. 2 is a flowchart showing a method for manufacturing the aluminum alloy material shown in FIG.
  • FIG. 3 is a cross-sectional view schematically showing a configuration of an aluminum alloy material according to a modification of the first embodiment of the present invention.
  • FIG. 4 is a flowchart showing a method for manufacturing the aluminum alloy material shown in FIG.
  • FIG. 5 is a cross-sectional view schematically showing a joined body according to the second embodiment of the present invention.
  • FIG. 6A is a side view schematically showing a test piece used for measurement of tensile shear strength.
  • FIG. 6B is a plan view schematically showing a test piece used for measurement of tensile shear strength.
  • FIG. 1 is a cross-sectional view schematically showing the configuration of the aluminum alloy material of the present embodiment.
  • an aluminum alloy material 10 of the present embodiment includes a first film 1 (hereinafter, referred to as an “oxidized film”) formed on at least a part of the surface of an aluminum alloy base material 3 (hereinafter also referred to as a base material 3).
  • a second film 2 (hereinafter also referred to as a film 2) having a siloxane bond is formed on at least a part of the first film 1.
  • the substrate 3 is made of an aluminum alloy.
  • the type of aluminum alloy that forms the base material 3 is not particularly limited, and various non-heat-treatable or heat-treated aluminums that are defined in JIS or approximate to JIS, depending on the use of the processed member. It can be used by appropriately selecting from alloys.
  • the non-heat treatment type aluminum alloy there are pure aluminum (1000 series), Al—Mn series alloy (3000 series), Al—Si series alloy (4000 series), and Al—Mg series alloy (5000 series).
  • the heat-treatable aluminum alloy there are an Al—Cu—Mg alloy (2000 series), an Al—Mg—Si alloy (6000 series), and an Al—Zn—Mg alloy (7000 series).
  • the base material 3 preferably has a 0.2% proof stress of 100 MPa or more from the viewpoint of strength.
  • Aluminum alloys that can form a base material that satisfies such characteristics include those containing relatively large amounts of magnesium, such as 2000 series, 5000 series, 6000 series, and 7000 series, and these alloys are necessary. Depending on the condition, it may be tempered. Among various aluminum alloys, it is preferable to use a 6000 series aluminum alloy because it has excellent age-hardening ability, has a relatively small amount of alloy elements, and is excellent in scrap recyclability and formability.
  • the first coating 1 is formed on at least a part of the surface of the substrate 3.
  • Mg is 0.1 atomic% or more and less than 20 atomic%
  • Si is 5 atomic% or more and 60 atomic% or less
  • Cu is 0%.
  • An oxide film containing less than 6 atomic% (an oxide film containing aluminum, hereinafter also referred to as “oxide film”).
  • the coating 1 is provided to increase the bonding strength and improve the adhesion durability.
  • the suitable range of each component amount contained in the film 1 will be described.
  • the first film 1 is formed on the entire surface of the base 3, but the present embodiment is not limited to this.
  • the first film 1 may be formed on only a part of the surface of the substrate 3.
  • the first film 1 may be formed on both surfaces of the base material 3.
  • the aluminum alloy constituting the base material of the aluminum alloy material usually contains magnesium (Mg) as an alloy component, and an oxide film that is a composite oxide of aluminum and magnesium is formed on the surface of the base material 3.
  • Mg magnesium
  • an adhesive resin such as an adhesive precoat layer is formed on the oxide film, the surface magnesium becomes a weak boundary layer of the adhesive interface, and the initial bonding strength decreases.
  • the Mg content in the oxide film is 20 atomic% or more, the bonding strength of the aluminum alloy material tends to decrease. Therefore, in the aluminum alloy material 10 of the present embodiment, the Mg content in the first film 1 made of an oxide film is restricted to less than 20 atomic%. Thereby, adhesion durability can be improved.
  • the Mg content of the film 1 is preferably less than 15 atomic% and more preferably less than 10 atomic% from the viewpoint of improving the adhesion durability.
  • the lower limit of the Mg content of the film 1 is set to 0.1 atomic% or more from the viewpoint of economy.
  • the Mg content in the film 1 can be measured by a high-frequency glow discharge optical emission spectrometry (GD-OES).
  • the method for adjusting the Mg content of the film 1 is not particularly limited.
  • an acid solution such as nitric acid, sulfuric acid and hydrofluoric acid, or an acidic solution such as mixed acid, or potassium hydroxide, sodium hydroxide, silicic acid.
  • a method of performing a surface treatment with an alkaline solution containing a salt and a carbonate can be applied. This method adjusts the Mg content of the film 1 (oxide film) by dissolving magnesium in an acid or alkali solution, and adjusts the treatment time, temperature, concentration and pH of the surface treatment solution.
  • the amount of Mg in the film 1 can be in the range described above.
  • Mg Even if Mg is contained to the extent of an impurity element, Mg may be concentrated in the film 1 when heat treatment is performed at a high temperature, and adjustment by surface treatment with acid or alkali is possible. Is necessary as appropriate. It is also possible to adjust the surface treatment chemical solution by containing Mg ions. Conditions for the treatment with the acidic solution can be appropriately set in consideration of the alloy composition of the base material 3, the thickness of the first coating 1, and the like, and are not particularly limited. For example, the pH is 2 or less, the treatment temperature is 10 to Conditions of 80 ° C. and processing time of 1 to 60 seconds can be applied.
  • the conditions for the treatment with the alkaline solution can be appropriately set in consideration of the alloy composition of the base material 3, the thickness of the oxide film 1, and the like, and are not particularly limited.
  • the pH is 10 or more and the treatment temperature is 10 to 10.
  • Conditions of 80 ° C. and processing time of 1 to 60 seconds can be applied.
  • Silicon (Si) has the effect of stabilizing the surface of the first film 1 and further has the effect of improving the adhesion with the second film 2 having a siloxane bond. For this reason, it is possible to suppress a decrease in bonding strength by including silicon in the first coating 1.
  • the Si content in the coating 1 is set to 5 to 60 atomic%.
  • the Si content in the film 1 is preferably 10 atomic% or more, and more preferably 15 atomic% or more. Further, from the viewpoint of spot weldability and uniformity of chemical conversion treatment, the Si content in the coating 1 is preferably 55 atomic percent or less, and more preferably 50 atomic percent or less.
  • a surface treatment with an acid or an alkali before forming the second film 2 similarly to the method described as a method for adjusting the Mg content.
  • Cu contained in the base material 3 is concentrated on the surface, and the first film 1 is formed.
  • Cu content increases.
  • the Cu content of the first coating 1 also increases when a large amount of Cu ions is contained in the treatment liquid such as the degreasing step and the pickling step.
  • the Cu content in the first coating 1 is restricted to less than 0.6 atomic%.
  • coat 1 is less than 0.5 atomic% from a viewpoint of an adhesive improvement with the membrane
  • the etching method is not limited.
  • a processing method similar to that described as a method for adjusting the amount of Mg can be applied. That is, for example, etching can be performed by treatment with an acid or alkali solution.
  • the element concentration such as Mg amount, Si amount, and Cu amount in the first film is measured by, for example, a high-frequency glow discharge emission spectroscopy (GD-OES: Glow Discharge-Optical Emission Spectroscopy). Can do.
  • GD-OES Glow Discharge-Optical Emission Spectroscopy
  • Mg, copper (Cu), iron (Fe), titanium (Ti) and other metal elements and silicon (Si) and other elements were measured, and the content of Mg, Si, Cu, etc. was calculated as a percentage. The value is the amount of each element.
  • the film thickness of the film 1 is preferably 1 to 30 nm.
  • the film thickness of the film 1 exceeds 30 nm, the amount of the film becomes excessive and irregularities are easily formed on the surface.
  • the surface of the coating 1 is uneven, for example, chemical conversion spots are likely to occur during the chemical conversion treatment performed before the coating process in automobile applications, leading to a decrease in chemical conversion.
  • the film thickness of the film 1 is more preferably 2 nm or more and less than 20 nm from the viewpoints of chemical conversion and productivity.
  • M is an element contained in the aluminum alloy substrate 3, specifically, Al and Mg contained in the coating 1.
  • This M—O—Si bond is a main bond between the first film 1 made of an oxide film and the second film 2 having a siloxane bond. It is influenced by the structure of the oxide film.
  • the amount of M—O—Si bonds is analyzed by Fourier transform infrared spectroscopy with parallel polarized light having an incident angle of 75 ° incident on the surface on which the first film 1 and the second film 2 are formed.
  • the spectrum obtained in this way can be obtained from the area of the peak derived from the M—O—Si bond generated in the vicinity of 1057 cm ⁇ 1 with 1026 cm ⁇ 1 to 1084 cm ⁇ 1 as the baseline. Note that the position of the peak derived from the M—O—Si bond is shifted in the range of about 1045 to 1065 cm ⁇ 1 depending on the type and ratio of M.
  • the area of the peak generated in the vicinity of 1057 cm ⁇ 1 calculated by the above-described method is 0.010 or more.
  • the area of the peak derived from this M—O—Si bond is less than 0.010, the ratio of occurrence of interfacial peeling at the interface between the first film 1 and the second film 2 increases, and the desired adhesion durability. You may not get sex.
  • the peak area derived from the M—O—Si bond is more preferably 0.012 or more, and further preferably 0.015 or more.
  • the second film 2 is a film containing a siloxane bond and formed on at least a part of the first film 1.
  • the second film 2 may be formed on the entire first film 1 or only on a part thereof.
  • the second film 2 is preferably formed thinly and uniformly on the film 1, but may be formed in an island shape on the film 1.
  • the second film 2 is a film containing siloxane bonds treated with a solution containing a silane coupling agent.
  • the amount of Si—O—Si bonds when the second film 2 having siloxane bonds is formed on the first film 1 greatly affects the durability of the bonding strength with the resin. Therefore, it is important to control the amount of Si—O—Si.
  • the amount of Si—O—Si bond is analyzed by Fourier transform infrared spectroscopy by entering parallel polarized light with an incident angle of 75 ° on the surface on which the first film 1 and the second film 2 are formed.
  • absorbance can be determined by the peak height in the vicinity of 1100cm -1 ⁇ 1140cm -1.
  • the first point and 400 cm -1 the extreme values of the highest frequency side of the extreme value (valley) in a second point between 1200cm -1 ⁇ 1300cm -1
  • a baseline is drawn and the peak height is obtained based on the baseline.
  • the peak height derived from this Si—O—Si bond is less than 0.01, the formation of the Si—O—Si network in the second film 2 becomes insufficient, so that the deterioration factor easily penetrates, and the resin The durability of the bonding strength tends to decrease, and the desired bonding strength durability cannot be obtained.
  • the peak height derived from the Si—O—Si bond is preferably 0.02 or more, and more preferably 0.05 or more.
  • the peak height derived from the Si—O—Si bond exceeds 0.50, the number of Si—O—Si bonds that can participate in the bond with the aluminum alloy material decreases, and the second film 2 and the first film It becomes easy to peel at the interface between 1. Therefore, in the aluminum alloy material 10 of the present embodiment, the peak height derived from the Si—O—Si bond is 0.50 or less, preferably 0.45 or less, and more preferably 0.40 or less.
  • the peak height derived from the Si—O—Si bond in the second film 2 can be controlled, for example, in the range of 0.01 to 0.50 as follows. That is, as one embodiment, after preparing a solution containing a silane coupling agent (hereinafter also referred to as a treatment liquid), the solution is allowed to stand for 5 minutes or more before being applied to the first film 1, and the treatment liquid is Si— An O—Si bond is easily formed. Subsequently, the treatment liquid may be applied to the first film 1, and drying may be started at 70 ° C. or higher within 10 minutes after application of the treatment liquid until the solvent is completely removed.
  • a solution containing a silane coupling agent hereinafter also referred to as a treatment liquid
  • the treatment liquid is allowed to stand for 5 minutes or more, more preferably 10 minutes or more, and even more preferably 15 minutes or more before being applied to the first film 1.
  • the treatment liquid is applied and left at room temperature for 10 minutes or more, self-polymerization proceeds, the Si—O—Si bond becomes excessive, and the bonding strength may be insufficient. Therefore, it is preferable to start drying within 10 minutes, more preferably within 8 minutes, and even more preferably within 5 minutes after applying the treatment liquid.
  • the drying temperature at the time of drying may be appropriately selected depending on the composition of the treatment liquid, but from the viewpoint of productivity, it is preferably 70 ° C. or higher, more preferably 75 ° C. or higher, and further preferably It is 80 ° C or higher. Further, from the viewpoint of surface quality, it is preferable to dry until the solvent is completely removed.
  • concentration of the silane coupling agent in the solution (processing liquid) containing a silane coupling agent is 0.01 mass% or more, for example, Preferably it is 0.1 mass% or more.
  • concentration of the silane coupling agent in a process liquid is 90 mass% or less, for example, Preferably it is 80 mass% or less.
  • the coating amount of the second coating 2 after drying can be adjusted as appropriate by adjusting the concentration of the treatment liquid and the coating amount.
  • the coating amount of the second coating 2 after drying is preferably adjusted to be 0.1 mg / m 2 or more and less than 30 mg / m 2 .
  • the coating amount of the second coating 2 after drying is 30 mg / m 2 or more, the second coating 2 itself may cause cohesive failure, resulting in a decrease in bonding strength.
  • the coating amount is less than 0.1 mg / m 2, the influence of Cu exposed on the surface of the substrate 3 and the amount of M—O—Si bond between the coating 1 and the coating 2 are insufficient. Adhesive durability may not be obtained.
  • silane coupling agent in the solution containing the silane coupling agent for forming the second film 2 examples include reactive functional groups such as amino group, epoxy group, methacryl group, methacryloxy group, vinyl group, and mercapto group.
  • the functional group of a silane coupling agent is not limited to what was mentioned above, The silane coupling agent which has various functional groups can be selected suitably, and can be used.
  • examples of the solvent used for the solution containing the silane coupling agent include organic solvents such as water and ethanol, or mixed solvents such as water and alcohol.
  • the method for applying the solution containing the silane coupling agent is not particularly limited, and an existing method can be applied. Specifically, a coating method by dipping, a method using various coating machines such as a roll coater, a bar coater, a gravure coater, a micro gravure coater, a reverse gravure coater, and a dip coater, a spray coating method, and the like can be applied.
  • FIG. 2 is a flowchart showing a method for manufacturing the aluminum alloy material 10 of the present embodiment. As shown in FIG. 2, when manufacturing the aluminum alloy material 10 of this embodiment, base material preparation process S1, 1st film formation process S2, and 2nd film formation process S3 are performed. Hereinafter, each step will be described.
  • the shape of the substrate is not particularly limited, and depending on the shape of a member produced using an aluminum alloy material, in addition to a plate shape, a cast material, a forged material, an extruded material (for example, a hollow bar shape), etc. Any shape that can be taken as In the base material manufacturing step S1, when a plate-shaped base material (substrate) is manufactured as an example, the substrate is manufactured by the following procedure, for example. First, an aluminum alloy having a predetermined composition is melted by continuous casting and cast to produce an ingot (melting casting process). Next, the produced ingot is subjected to homogenization heat treatment (homogenization heat treatment step).
  • the ingot subjected to homogenization heat treatment is hot-rolled to produce a hot-rolled sheet (hot-rolling step).
  • the hot-rolled sheet is subjected to rough annealing or intermediate annealing at 300 to 580 ° C., and cold rolling with a final cold rolling rate of 5% or more is performed at least once, so that a cold-rolled sheet (substrate) having a predetermined thickness is obtained. (Cold rolling process).
  • the temperature of rough annealing or intermediate annealing it is preferable to set the temperature of rough annealing or intermediate annealing to 300 ° C. or higher, and thereby the effect of improving formability is more exhibited.
  • the temperature of rough annealing or intermediate annealing shall be 580 degrees C or less, and this becomes easy to suppress the fall of the moldability by generation
  • the final cold rolling rate is preferably 5% or more, and thereby, the effect of improving the formability is more exhibited.
  • the conditions of homogenization heat processing and hot rolling are not specifically limited, It can carry out on the conditions in the case of obtaining a hot rolled sheet normally. Further, intermediate annealing may not be performed.
  • Step S2 First film formation step>
  • the first film 1 made of an oxide film is formed on at least a part of the surface of the substrate 3 produced in the substrate production process of step S1. .
  • the formed oxide film is surface-treated so that the Mg amount, the Si amount, and the Cu amount are in specific ranges, respectively.
  • the base material 3 is heated to 400 to 580 ° C., for example, to form an oxide film constituting the first film 1 on the surface of the base material 3. Further, the heat treatment also has an effect of adjusting the strength of the aluminum alloy material 10.
  • the heat treatment performed here is a solution treatment when the substrate 3 is formed of a heat-treatable aluminum alloy, and is annealed when the substrate 3 is formed of a non-heat-treatable aluminum alloy. It is heat processing in (final annealing).
  • This heat treatment is preferably rapid heating at a heating rate of 100 ° C./min or more from the viewpoint of improving the strength.
  • the strength of the aluminum alloy material 10 and the strength after heating (baking) of the aluminum alloy material 10 can be further increased by setting the heating temperature to 400 ° C. or higher and performing rapid heating.
  • the heating temperature is set to 580 ° C. or less and performing rapid heating, it is possible to suppress a decrease in formability due to the occurrence of burning.
  • the holding time in the heat treatment is preferably 3 to 30 seconds.
  • the surface treatment of the oxide film formed by the above-described method is performed so that the Mg amount, Si amount, and Cu amount in the film 1 are in a specific range.
  • the specific surface treatment method since the specific surface treatment method has already been mentioned above, detailed description is abbreviate
  • the oxide film structure control which affects the amount of Mg in the 1st membrane
  • the heat treatment which is an aluminum alloy component and a previous process also indirectly affects the amount of these components and the oxide film structure, it is necessary to appropriately adjust the treatment conditions.
  • step S2 although adjustment of Mg amount in the 1st film
  • Step S3 Second film forming step>
  • the second film 2 having a siloxane bond is formed as a second film forming process (second film forming process).
  • a solution containing a silane coupling agent prepared and allowed to stand for 5 minutes or more is applied to at least a part of the first film, and within 10 minutes after the application of the solution. Dry at a temperature of 70 ° C. or higher.
  • the peak height derived from the Si—O—Si bond in the second film 2 can be controlled to 0.01 or more and 0.50 or less.
  • ⁇ Other processes> In the manufacturing process of the aluminum alloy material 10 of the present embodiment, other processes may be included between or before and after each process as long as the processes described above are not adversely affected.
  • This preliminary aging treatment is preferably performed by heating at 40 to 120 ° C. within 72 hours at a low temperature of 8 to 36 hours.
  • pre-aging treatment By performing pre-aging treatment under these conditions, it is possible to improve moldability and strength after baking.
  • a foreign matter removing step for removing foreign matter on the surface of the aluminum alloy material 10 or a defective product removing step for removing defective products generated in each step may be performed.
  • the manufactured aluminum alloy material 10 is coated with press oil on the surface thereof before the fabrication of the joined body or before processing into the member for an automobile.
  • the press oil one containing an ester component is mainly used.
  • the method and conditions for applying the press oil to the aluminum alloy material 10 are not particularly limited, and methods and conditions for applying the normal press oil can be widely applied.
  • a press containing ethyl oleate as an ester component What is necessary is just to immerse the aluminum alloy material 10 in oil.
  • the ester component is not limited to ethyl oleate, and various materials such as butyl stearate and sorbitan monostearate can be used.
  • the aluminum alloy material 10 of the present embodiment includes an oxide film (film 1) containing a specific amount of Mg, the elution of the base material 3 can be suppressed, and the surface of the base material 3 associated therewith. It is possible to suppress the alkalinization of the resin and to suppress the deterioration of the adhesive resin. Furthermore, since the coating 1 contains a specific amount of Si and the amount of Cu in the coating 1 is regulated to be less than the specific amount, the adhesion between the coating 1 and the coating 2 is improved.
  • the aluminum alloy material 10 of this embodiment in the spectrum obtained by making parallel polarized light with an incident angle of 75 ° incident on the surface on which the coating 1 and the coating 2 are formed by Fourier transform infrared spectroscopy, 1100 cm Since the peak height in the vicinity of ⁇ 1 to 1400 cm ⁇ 1 is adjusted to be 0.01 or more and 0.50 or less, the durability of the bonding strength is excellent. As a result, the aluminum alloy material 10 of the present embodiment is excellent in productivity, has high bonding strength, and does not easily decrease the bonding strength.
  • FIG. 3 is a cross-sectional view schematically showing the configuration of the aluminum alloy material of this modification.
  • the same components as those of the aluminum alloy material 10 shown in FIG. 1 are denoted by the same reference numerals, and detailed description thereof is omitted.
  • the aluminum alloy material 11 of this modification is a thermoplastic resin so as to cover the first film 1 and the second film 2 of the aluminum alloy substrate 3 of the first embodiment described above.
  • An adhesive precoat layer 4 containing is formed. The aluminum alloy material 11 of this modification can be bonded to the resin material via the adhesive precoat layer 4.
  • the adhesive precoat layer 4 contains a thermoplastic resin. By configuring the adhesive precoat layer 4 to include a thermoplastic resin, when the aluminum alloy material and the resin material are bonded, the molding of the resin material and the bonding with the resin material can be performed at the same time. In addition, the manufacturing cost can be suppressed.
  • the adhesive precoat layer 4 may be formed on the entire portion where the first film 1 and the second film 2 are formed, or the first film 1 and the second film 2 are formed. It may be formed only on a part of the portion.
  • the thermoplastic resin used for the adhesive precoat layer 4 is selected from, for example, polyolefins such as ethylene vinyl acetate (EVA), polyurethane, polyester polyethylene, and polypropylene, and polyamides such as nylon 6, nylon 66, and nylon 12. 1 type (s) or 2 or more types can be used.
  • the thermoplastic resin may be acid-modified, or may be used by being dispersed in a resin-based paint having good adhesiveness.
  • the thickness of the adhesive precoat layer 4 is not particularly limited, but if it is less than 1 ⁇ m, desired bonding strength may not be obtained. Therefore, the thickness of the adhesive precoat layer 4 is preferably 1 ⁇ m or more, more preferably 3 ⁇ m or more. On the other hand, if the thickness of the adhesive precoat layer 4 exceeds 100 ⁇ m, cohesive failure may occur, and the cost increases. Therefore, the thickness of the adhesive precoat layer 4 is preferably 100 ⁇ m or less, and more preferably 90 ⁇ m or less.
  • FIG. 4 is a flowchart showing a method for manufacturing the aluminum alloy material 11 of this modification. As shown in FIG. 4, when the aluminum alloy material 11 of the present modification is manufactured, an adhesive precoat layer forming step S4 is performed in addition to the steps S1 to S3 described above.
  • Step S4 Adhesive precoat layer forming step
  • the adhesive precoat layer 4 is formed so as to cover the first film 1 and the second film.
  • the method for forming the adhesive precoat layer 4 is not particularly limited.
  • a dispersion or solution of a thermoplastic resin is applied by spray coating, dip coating, electrostatic coating, roll coating coating, or the like. And drying and heat treatment.
  • attachment precoat layer 4 can be formed by performing a lamination, a hot press, etc.
  • the thickness of the adhesive precoat layer 4 can be adjusted by appropriately selecting the solid component concentration or solution concentration of the thermoplastic resin dispersion or solution, the coating amount, the film thickness, and the like.
  • the second film forming step S3 and / or the adhesive precoat layer forming step S4 You may provide the preliminary aging treatment process which performs an aging treatment.
  • the adhesive precoat layer 4 is provided in advance, and therefore, operations such as providing an adhesive precoat layer on the surface of the aluminum alloy material are omitted when a joined body or an automobile member is manufactured. be able to.
  • the configuration and effects of the aluminum alloy material of this modification other than those described above are the same as those in the first embodiment described above.
  • the aluminum alloy material 11 of this modification may be joined to the resin material via the adhesive precoat layer 4, it may be joined to other members other than the resin material.
  • other members as in the case of the aluminum alloy material 11, another aluminum alloy material on which the first film and the second film are formed, the first film, and the second film are formed. Aluminum alloy materials that are not used are included.
  • FIG. 5 is a cross-sectional view schematically showing a configuration example of the joined body of the present embodiment.
  • the same components as those of the aluminum alloy material 11 shown in FIG. 3 are denoted by the same reference numerals, and detailed description thereof is omitted.
  • the resin material 5 is joined to the adhesive precoat layer 4 side of the aluminum alloy material 11 provided with the adhesive precoat layer 4 shown in FIG. 3.
  • the resin for forming the resin material 5 used in the bonded body 21 is not particularly limited.
  • polyolefin such as polypropylene, nylon 6, nylon 6, 6, polyamide such as aromatic nylon, polystyrene, polyurethane, and acrylonitrile.
  • ABS butadiene / styrene copolymer resin
  • POM polyoxymethylene
  • PC polycarbonate
  • PET polyethylene terephthalate
  • PPS polyphenylene sulfide
  • thermoplastic resin capable of compression molding such as injection molding or hot pressing is preferable.
  • a reinforcing material such as glass fiber, carbon fiber, aramid fiber, plant-derived fiber, metal fiber, silica, talc, calcium carbonate, mica may be added to the resin material 5 in accordance with required characteristics. .
  • the joined body 21 shown in FIG. 5 since one surface of the adhesive precoat layer 4 is joined to the coating 1 and the coating 2 side, when it is used for an automobile member, it has high joining strength and the joining strength does not easily decrease. It becomes. Moreover, since the joined body 21 shown in FIG. 5 is bonded to the aluminum alloy material 11 and the resin material 5, the joined body 21 is lighter than the joined body of the aluminum alloy materials. Further weight reduction can be realized.
  • a method for joining the aluminum alloy material 11 and the resin material 5 in manufacturing the joined body 21 is not particularly limited, and a conventionally known joining method can be used.
  • examples of such methods include compression molding methods such as injection molding of molten resin, SMC (Sheet Molding Compound) molding, and BMC (Bulk Molding Compound) molding.
  • compression molding methods such as injection molding of molten resin, SMC (Sheet Molding Compound) molding, and BMC (Bulk Molding Compound) molding.
  • RTM Resin Transfer Molding
  • VaRTM Vauum Assisted Resin Transfer Molding
  • HP-RTM High Pressure-Resin Transfer Molding
  • LFT-D Lt-Frm-Ltr-Dr-Frm-Lt-Frm-Lt-Frm-Lt-Frm-Lt-Fr-Dr Good.
  • Resin molding for forming the resin material 5 is performed by molding the resin for forming the resin material 5 in a state where the aluminum alloy material 11 is disposed in the mold used for molding the resin for forming the resin material 5.
  • the material 5 and the aluminum alloy material 11 can be joined at the same time, and excellent productivity and cost reduction can be achieved.
  • the injection molding, the injection compression molding, the compression molding and the LFT-D method are preferable because of excellent productivity.
  • a heat treatment may be performed at a temperature of 80 ° C. or more for 3 minutes or more.
  • the bonding strength and the durability of the bonding strength can be further improved. This is because the amount of interface bonding between the second film 2 and the adhesive precoat layer 4 is further increased by the heat treatment, and the initial adhesive strength is improved.
  • the heat treatment suppresses the penetration of deterioration factors, makes it difficult for the Si—O—Si bond to be broken, and improves the durability of the bonding strength.
  • the heating temperature when the heat treatment is performed is preferably 80 ° C. or higher, more preferably 85 ° C. or higher, and still more preferably 90 ° C. or higher, from the viewpoint of obtaining the above effects satisfactorily.
  • the heating temperature exceeds the melting point of the resin constituting the resin material 5 to be joined or the melting point of the resin constituting the adhesive precoat layer 4, the shape may become unstable, and thus the temperature does not exceed these melting points. It is preferable.
  • the heating time in the case of performing the heat treatment is preferably 3 minutes or more, more preferably 5 minutes or more, and further preferably 10 minutes or more from the viewpoint of obtaining the above effects satisfactorily.
  • the heating time is preferably 200 hours or less, more preferably 150 hours or less, and even more preferably 100 hours or less.
  • the heat treatment may be performed again after returning to normal temperature after the heat treatment.
  • the heating conditions such as heating temperature and heating time when the heat treatment is performed a plurality of times may be the same or different at each time.
  • a cooling treatment for 3 minutes or more may be further performed at a temperature below the freezing point in combination with a heat treatment for 3 minutes or more at a temperature of 80 ° C. or higher.
  • the cooling temperature in the case of performing the cooling treatment is preferably a temperature below freezing point, more preferably ⁇ 5 ° C. or less, and still more preferably ⁇ 10 ° C. or less, from the viewpoint of obtaining the above effect satisfactorily.
  • the cooling temperature is preferably ⁇ 80 ° C. or higher.
  • the cooling time when performing the cooling treatment is preferably 3 minutes or more, more preferably 5 minutes or more, and even more preferably 10 minutes or more, from the viewpoint of obtaining the above effects satisfactorily.
  • the cooling temperature is preferably 200 hours or less, more preferably 150 hours or less, and even more preferably 100 hours or less.
  • the heating conditions such as the cooling temperature and the cooling time when the cooling treatment is performed a plurality of times may be the same each time or may be different.
  • either the cooling treatment or the heat treatment may be performed first, or the cooling treatment and the heat treatment may be alternately repeated. Furthermore, after performing either one of a cooling process and a heat processing continuously several times, you may perform the other.
  • the joined body 21 may be coated with press oil on the surface thereof before being processed into a member for an automobile.
  • the member for motor vehicles of this embodiment uses the joined object of a 2nd embodiment mentioned above, for example, is a panel for motor vehicles.
  • the automobile member of the present embodiment is manufactured from the joined body of the second embodiment described above, it has excellent productivity and high joint strength, and the joint strength is not easily lowered.
  • the metal surface was treated by the following methods and conditions, and adhesion durability and the like were evaluated.
  • Each joined body according to each example (No. 1 to 17) was produced by the method shown below.
  • No. Nos. 1 to 6 are comparative examples.
  • Examples 7 to 17 are examples.
  • no. About No. 1 it processed for 30 second with the 60 degreeC alkali degreasing agent adjusted to pH10 or more.
  • No. 2 was treated for 30 seconds with a 60 ° C. alkaline degreasing agent adjusted to pH 10 or higher, and then treated for 10 seconds with a 50 ° C. pickling solution containing sulfuric acid adjusted to pH 2 or lower.
  • No. 3 was treated with an alkaline degreasing agent at 60 ° C. adjusted to pH 10 or higher for 30 seconds, and then treated with pickling solution at 50 ° C. containing sulfuric acid adjusted to pH 2 or lower for 60 seconds.
  • the base material of each example was washed with water within 5 minutes after the above treatment, and dried within 5 minutes after washing with water to form a first film which was an oxide film.
  • the silane coupling agent aqueous solution obtained by diluting an amino group-containing silane coupling agent (KBE903, manufactured by Shin-Etsu Chemical Co., Ltd.) with pure water is formed on the first film on the substrate.
  • the film was dried to form a second film, and an aluminum alloy material was produced.
  • the coating amount after drying was controlled by changing the dilution rate of the silane coupling agent aqueous solution and the count of the bar coater.
  • Adhesive precoat layer forming step Furthermore, a paint-based adhesive primer containing nylon resin is applied to the surface of the base material on which the first film and the second film are formed with a bar coater and dried at 170 ° C. for 5 minutes to form an adhesive precoat layer. It was. After drying, the aluminum alloy material was cut into a length of 100 mm and a width of 50 mm. At this time, the thickness of the adhesive precoat layer after drying in each example was adjusted to the value shown in Table 1 by adjusting the count of the bar coater.
  • the aluminum alloy material 31a is placed in a mold of an injection molding machine capable of producing a test piece as shown in FIGS. 6A and 6B, and the resin material 31b is injection molded of nylon 6 containing 30% glass fiber, and a resin.
  • the material 31b and the aluminum alloy material 31a were joined at the same time. At this time, the mold temperature of the injection molding machine was 70 ° C.
  • Heat treatment process No. For 10 to 16, heat treatment processes were performed on the prepared test pieces under the conditions shown in Table 1.
  • the first film component was measured for the base material before forming the second film. Specifically, the first film was measured while being sputtered in the film thickness direction by high-frequency glow discharge optical emission spectrometry (GD-OES: model JY-5000RF manufactured by Horiba Joban Yvon), aluminum (Al), Metal elements such as magnesium (Mg), copper (Cu), iron (Fe) and titanium (Ti), and oxygen (O), nitrogen (N), carbon (C), silicon (Si), sulfur (S), etc. The amount of each component was measured for these elements.
  • GD-OES model JY-5000RF manufactured by Horiba Joban Yvon
  • Metal elements such as magnesium (Mg), copper (Cu), iron (Fe) and titanium (Ti), and oxygen (O), nitrogen (N), carbon (C), silicon (Si), sulfur (S), etc.
  • the amount of each component was measured for these elements.
  • the maximum concentration of magnesium (Mg), copper (Cu) and silicon (Si) in the oxide film was defined as the film concentration in the film. Since aluminum (Al) is affected by the base material in the vicinity of the interface between the base material and the first film, the concentration of the outermost surface is the aluminum (Al) film concentration.
  • oxygen (O) and carbon (C) are particularly susceptible to contamination on the outermost surface and in the vicinity thereof. From the above, in the concentration calculation of each element, the concentration was calculated excluding oxygen (O) and carbon (C).
  • oxygen (O) is highly likely to be affected by contamination at the outermost surface and in the vicinity thereof, and it is difficult to measure the exact concentration, but oxygen (O) is present in the first film of all samples. It was clear that it was included. The measurement results in each example are shown in Table 1.
  • the Si—O—Si bond amount was analyzed for the aluminum alloy material before forming the adhesive precoat layer. Specifically, the amount of Si—O—Si bonds is determined by the incidence of parallel polarized light with an incident angle of 75 ° on the surface on which the first film and the second film are formed, by Fourier transform infrared spectroscopy. in the case where a spectrum obtained by analyzing the displayed absorbance was determined by peak height in the vicinity of 1100cm -1 ⁇ 1140cm -1.
  • test pieces prepared in each example were stored in a desiccator for one day or longer, the tensile shear strength (initial bonding strength) was measured with a universal testing machine. Moreover, after the test piece produced in each example was stored in a desiccator for one day or more and further immersed in hot water at 70 ° C. for 200 hours, the tensile shear strength (joining strength after water resistance test) was measured with a universal testing machine.
  • the case where the tensile shear strength is less than 2 MPa is “x”, the case where it is 2 MPa or more and less than 5 MPa is “ ⁇ ”, the case where it is 5 MPa or more but less than 10 MPa is “ ⁇ ”, the case where it is 10 MPa or more but less than 20 MPa is “ ⁇ ”, 20 MPa
  • the above cases were evaluated as “ ⁇ ”.
  • the evaluation results in each example are shown in Table 1.
  • the case where an evaluation result was " ⁇ ", " ⁇ ", or " ⁇ ” was evaluated as acceptable, and the case where the evaluation result was " ⁇ " or " ⁇ ” was evaluated as unacceptable.
  • any of Mg, Si, Cu, and Si—O—Si bonds is out of the range specified in the present invention.
  • the evaluations of the initial bonding strength and the bonding strength after the water resistance test were both “x” or “ ⁇ ”, the bonding strength was low, and the durability of the bonding strength was poor.
  • No. which is an embodiment of the present invention In Nos. 7 to 17, the initial joint strength and the joint strength evaluation after the water resistance test are all “ ⁇ ”, “ ⁇ ”, or “ ⁇ ”, and the joint strength is high and the durability of the joint strength is excellent. there were.
  • No. 1 in which the thickness of the adhesive precoat layer is in the range of 1 to 100 ⁇ m. 7 and no. In 9 to 17, the adhesive strength was further improved.

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Abstract

La présente invention concerne un matériau d'alliage d'aluminium, lequel matériau comporte : un matériau de base en alliage d'aluminium ; un premier film qui comprend un film d'oxyde ne contenant pas moins de 0,1 %en pourcentage atomique mais moins de 20,0 %en pourcentage atomique de Mg, 5 à 60 %en pourcentage atomique de Si, et moins de 0,6 %en pourcentage atomique de Cu, et qui est formé au moins sur une partie de la surface du matériau de base en alliage d'aluminium ; et un second film contenant une liaison siloxane qui est formé sur au moins une partie du premier film, et, dans un spectre obtenu à l'aide d'une spectroscopie à infrarouges à transformée de Fourier par le fait d'amener une lumière polarisée parallèle ayant un angle d'incidence de 75° à être incidente sur une surface sur laquelle les premier et second films sont formés, la hauteur d'un pic dans le voisinage de 1100 à 1400 cm-1 étant de 0,01 à 0,50.
PCT/JP2016/074628 2015-09-02 2016-08-24 Matériau d'alliage d'aluminium, corps lié, élément d'automobile, procédé pour produire un matériau d'alliage d'aluminium, et procédé pour produire un corps lié Ceased WO2017038573A1 (fr)

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JP2016035807A JP2017048456A (ja) 2015-09-02 2016-02-26 アルミニウム合金材、接合体、自動車用部材、アルミニウム合金材の製造方法及び接合体の製造方法

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998056577A1 (fr) * 1997-06-12 1998-12-17 Toyo Kohan Co., Ltd. Feuille d'alliage d'aluminium a revetement de resine pour couvercles de boites
JP2003147550A (ja) * 2001-07-23 2003-05-21 Mitsubishi Alum Co Ltd 表面処理アルミニウム缶用板材
JP2013166975A (ja) * 2012-02-14 2013-08-29 Kobe Steel Ltd 表面処理アルミニウム合金板およびその製造方法
JP2015003514A (ja) * 2013-05-23 2015-01-08 株式会社神戸製鋼所 アルミニウム合金板、接合体及び自動車用部材
JP2015157967A (ja) * 2014-02-21 2015-09-03 株式会社神戸製鋼所 アルミニウム合金板、接合体及び自動車用部材
WO2016076344A1 (fr) * 2014-11-11 2016-05-19 株式会社神戸製鋼所 Matériau alliage d'aluminium, corps collé, élément pour automobiles, et procédé de production du matériau alliage d'aluminium

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998056577A1 (fr) * 1997-06-12 1998-12-17 Toyo Kohan Co., Ltd. Feuille d'alliage d'aluminium a revetement de resine pour couvercles de boites
JP2003147550A (ja) * 2001-07-23 2003-05-21 Mitsubishi Alum Co Ltd 表面処理アルミニウム缶用板材
JP2013166975A (ja) * 2012-02-14 2013-08-29 Kobe Steel Ltd 表面処理アルミニウム合金板およびその製造方法
JP2015003514A (ja) * 2013-05-23 2015-01-08 株式会社神戸製鋼所 アルミニウム合金板、接合体及び自動車用部材
JP2015157967A (ja) * 2014-02-21 2015-09-03 株式会社神戸製鋼所 アルミニウム合金板、接合体及び自動車用部材
WO2016076344A1 (fr) * 2014-11-11 2016-05-19 株式会社神戸製鋼所 Matériau alliage d'aluminium, corps collé, élément pour automobiles, et procédé de production du matériau alliage d'aluminium

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