WO2011071062A1 - Composite d'aluminium lie et son procede de fabrication - Google Patents

Composite d'aluminium lie et son procede de fabrication Download PDF

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Publication number
WO2011071062A1
WO2011071062A1 PCT/JP2010/071973 JP2010071973W WO2011071062A1 WO 2011071062 A1 WO2011071062 A1 WO 2011071062A1 JP 2010071973 W JP2010071973 W JP 2010071973W WO 2011071062 A1 WO2011071062 A1 WO 2011071062A1
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WIPO (PCT)
Prior art keywords
aluminum
adhesive
shaped body
composite material
adhesive layer
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PCT/JP2010/071973
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English (en)
Japanese (ja)
Inventor
令子 高澤
正憲 遠藤
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日本軽金属株式会社
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Priority to CN2010800558639A priority Critical patent/CN102652059A/zh
Publication of WO2011071062A1 publication Critical patent/WO2011071062A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
    • C09J5/02—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving pretreatment of the surfaces to be joined
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2400/00—Presence of inorganic and organic materials
    • C09J2400/10—Presence of inorganic materials
    • C09J2400/16—Metal
    • C09J2400/163—Metal in the substrate
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2400/00—Presence of inorganic and organic materials
    • C09J2400/10—Presence of inorganic materials
    • C09J2400/16—Metal
    • C09J2400/166—Metal in the pretreated surface to be joined
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2400/00—Presence of inorganic and organic materials
    • C09J2400/20—Presence of organic materials
    • C09J2400/22—Presence of unspecified polymer

Definitions

  • the present invention relates to an aluminum-adhesive composite material in which a metal or resin adherend is integrally bonded to the surface of an aluminum shape body made of aluminum or an aluminum alloy via an adhesive layer, and a method for producing the same.
  • the present invention relates to an aluminum adhesive composite material excellent in bonding strength that can be suitably used in the field, and a method for producing the same.
  • Patent Document 1 discloses an aluminum core metal foil characterized in that a metal foil is bonded to aluminum or an aluminum alloy having a surface roughness (Rmax) of about 8 to 18 ⁇ m via an organic resin or an organic-inorganic composite resin. A tension laminate has been proposed.
  • Patent Document 2 the surface of the aluminum plate to be laminated polyamide sheet, after the epoxy silane coupling agent 1 ⁇ 100 mg / m 2 was applied, polyamide laminate, characterized by heating and melting superimposed polyamide sheet A method for manufacturing an aluminum plate has been proposed.
  • Patent Document 3 is characterized in that a metal shaped article is immersed in an aqueous solution containing a water-soluble reducing agent, the metal shaped article pulled up from the aqueous solution is washed with water, dried and used as an adhesive. Metal bonding methods have been proposed.
  • Patent Document 4 there is a roughness on the order of microns due to chemical etching, and the surface is covered with fine irregularities with an irregular period of 5 to 500 nm, and the surface is A metal component that is a thin layer of a metal oxide or a metal phosphate, an adherend that is adhesively bonded to the metal component, and one liquid that is applied to the bonding surface of the metal component and the adherend to bond them together
  • An adhesive composite containing a metal alloy characterized by comprising an adhesive layer that is a cured product of a heat-curable thermosetting resin adhesive has been proposed.
  • the inventors of the present invention are an aluminum bonded composite material in which a metal or resin adherend is integrally bonded to the surface of an aluminum shape body made of aluminum or aluminum alloy via an adhesive layer.
  • the etching process has improved the shape of the aluminum body. It has been found that the bonding strength between the aluminum shaped body and the adhesive layer is remarkably improved by forming a specific surface shape having a concave portion on the surface, and the present invention has been completed.
  • an object of the present invention is to provide an aluminum-adhesive composite material in which an aluminum-shaped body made of aluminum or an aluminum alloy and an adherend made of metal or resin are integrally bonded via an adhesive layer. It is an object of the present invention to provide an aluminum-adhesive composite material that has extremely high bonding strength at the interface between the adhesive layer and the adhesive layer, and can exhibit excellent durability.
  • Another object of the present invention is to provide an aluminum bonded composite material in which an aluminum shape body made of aluminum or an aluminum alloy and a metal or resin bonded object are integrally bonded via an adhesive layer.
  • An object of the present invention is to provide a method for producing an aluminum-adhesive composite material that has extremely high bonding strength at the interface between a shaped body and an adhesive layer and can exhibit excellent durability.
  • the present invention provides an aluminum or aluminum alloy-made aluminum body having a concavo-convex portion on a part or the entire surface thereof, a metal or resin adherend that is located on the surface side of the aluminum body, and these An aluminum-adhesive composite material comprising an adhesive layer located between the aluminum-shaped body and the adherend and integrally bonding between the aluminum-shaped body and the adherend, and the surface of the aluminum-shaped body Are formed with a plurality of concave portions due to the concave and convex portions, and in the concave portions, there are formed fitting portions of an adhesive layer into which the adhesive has entered and solidified, and are fitted with the concave portions. An aluminum-adhesive composite material in which the aluminum shaped body and the adhesive layer are locked to each other by the portion.
  • the present invention also provides an aluminum or aluminum alloy-made aluminum body having a concavo-convex portion on a part of or the entire surface thereof, a metal or resin adherend that is located on the surface side of the aluminum body, and these An aluminum-adhesive composite material comprising an adhesive layer located between the aluminum-shaped body and the adherend and integrally bonding between the aluminum-shaped body and the adherend, and the surface of the aluminum-shaped body
  • An aluminum-adhesive composite material comprising an adhesive layer located between the aluminum-shaped body and the adherend and integrally bonding between the aluminum-shaped body and the adherend, and the surface of the aluminum-shaped body
  • a plurality of concave portions are formed due to the concave and convex portions, and each concave portion is orthogonal to the thickness direction in the thickness direction cross section of the aluminum-shaped body, and the highest portion of the concave and convex portions is formed.
  • the opening width measured by scanning electron microscope observation is 0.1 ⁇ m or more and 30 ⁇ m or less, and the depth is 0 .1 ⁇ m or more
  • These concave portions are formed with insertion portions of an adhesive layer in which the adhesive has entered and solidified during the bonding, and are bonded to the aluminum body by the concave portions and the insertion portions.
  • the aluminum adhesive composite material is characterized in that the agent layers are locked to each other.
  • the aluminum shape body made from aluminum or aluminum alloy which has an uneven
  • an aluminum shape body having a plurality of concave portions due to the concavo-convex portions is formed on a part or the entire surface of the surface, and an adherend is bonded to the surface of the aluminum shape body with an adhesive.
  • the adhesive enters into each concave portion of the aluminum-shaped body to form a fitting portion of the adhesive layer, and the concave portion of the aluminum-shaped body and the fitting portion of the adhesive layer are locked to each other to form the aluminum-shaped body.
  • the adhesive layer It is a manufacturing method of an aluminum adhesive composite material, characterized in that to produce the body-specifically bound aluminum adhesive composite.
  • examples of the aluminum or aluminum alloy material for forming the aluminum shaped body include a rolled material, an extruded shape material, a die-cast material, and a casting material.
  • the plurality of concave portions formed on the surface of the aluminum shape body due to the uneven portions on the surface of the aluminum shape body have a hole shape or an opening edge portion which is an endless peripheral portion. It may be a hole (a concave part having an endless opening edge), or a slit or groove having an opening edge having both ends (a concave part having an end opening edge) Further, a hole-like or hole-like one having these endless opening edges and a slit-like or groove-like one having endless opening edges may be mixed.
  • the protrusion part protruded in the shape of a snow flake toward the opening width direction center from a part or all part of the opening edge part of a recessed part preferably is formed.
  • the opening width of the concave portion is narrower than the width of the inside of the concave portion, and the insertion portions of the adhesive layer that has entered and solidified into the concave portion are mutually connected to the concave portion.
  • a non-releasable locking structure is formed, and it does not detach unless one or both of the concave portion of the aluminum shape body or the fitting portion of the adhesive layer is destroyed, and the aluminum shape body and the adhesive layer The bonding strength between them is further improved.
  • the opening width (d) measured by observation with a scanning electron microscope is 0.1 ⁇ m or more and 30 ⁇ m or less, preferably 0.5 ⁇ m or more and 20 ⁇ m or less, more preferably 1 ⁇ m or more and 10 ⁇ m or less, and the depth is 0.
  • the size may be 1 ⁇ m or more and 30 ⁇ m or less, preferably 0.5 ⁇ m or more and 20 ⁇ m or less.
  • the opening width (d) of the concave portion is smaller than 0.1 ⁇ m, it is difficult for the adhesive to enter when the adhesive is applied, and a fine void is generated at the interface between the aluminum body 1 and the adhesive layer.
  • the dissolution reaction proceeds excessively during the surface treatment (etching treatment) of the aluminum shaped body 1, and the material surface is missing or the thickness of the material is reduced. The problem of an increase occurs, and a product with insufficient material strength is generated, causing a decrease in productivity.
  • the depth is less than 0.1 ⁇ m, it is difficult to obtain a sufficient adhesive layer insertion portion. Conversely, if the depth is more than 30 ⁇ m, the surface treatment (etching treatment) of the aluminum shaped body 1 is performed. The dissolution reaction proceeds excessively, resulting in a problem that the surface of the material is missing or the thickness reduction amount of the material is increased.
  • the density of the plurality of concave portions formed due to the concave and convex portions on the surface of the aluminum-shaped body is in the range of an opening width of 0.5 ⁇ m to 20 ⁇ m and a depth of 0.5 ⁇ m to 20 ⁇ m per 0.1 mm square. It is preferable that one or two or more of them have a size of about 5 to 200.
  • the snow candy-like protrusion formed in the concave portion is preferably from the adhesive layer side to the aluminum shape body side in the cross section in the thickness direction of the aluminum adhesive composite material.
  • the thickness of the aluminum-shaped body portion of the laminated portion is preferably in the range of 0.1 ⁇ m or more and 30 ⁇ m or less, and the aluminum adhesive composite material has such a snow ridge-like protrusion within the range of 1000 observation lines. There should be more than one.
  • the plurality of concave portions of the aluminum-shaped body may have a double concave portion structure in which at least one or more internal concave portions are formed on the inner wall surface in part or all of the concave portions, It may have an internal concavo-convex structure in which at least one or more internal protrusions are formed on the inner wall surface, and these double concave structure and internal concavo-convex structure may coexist.
  • the presence of such a double concave portion structure or internal concavo-convex structure makes it possible for the concave portion of the aluminum shape body and the fitting portion of the adhesive layer to be more mutually connected. It bonds firmly and exhibits better bonding strength between the aluminum shaped body and the adhesive layer.
  • an aluminum-shaped body having a plurality of desired concave portions as described above is formed on the surface.
  • an aluminum alloy material is used as the method.
  • An etching process is performed to form a concavo-convex portion on part or the entire surface, and an aluminum shape body having a plurality of concave portions due to the concavo-convex portion is formed.
  • Etching solutions used for etching the aluminum alloy material include, for example, hydrochloric acid, phosphoric acid, sulfuric acid, acetic acid, oxalic acid, ascorbic acid, benzoic acid, butyric acid, citric acid, formic acid, lactic acid, isobutyric acid, apple
  • An etching solution composed of an acid aqueous solution such as acid, propionic acid, and tartaric acid can be mentioned, but a plurality of concave portions having a desired opening width and depth, or a part of the concave portion or In order to control the concave part formed on the surface to the desired shape and size, such as forming a snow squirrel-shaped protrusion projecting toward the center of the opening width direction on all opening edges, it is compared with an acid aqueous solution.
  • An etching solution containing the above halogen ions in a predetermined concentration range is preferably used. Then, using such an aqueous acid solution containing a relatively weak oxidizing power containing halogen ions, and immersing the aluminum alloy material in this etching solution, the halogen ions in the etching solution first dissolve the oxide film on the surface of the aluminum alloy material. After that, the inner aluminum alloy is melted and further eroded into the aluminum alloy material.
  • the inner aluminum alloy is more easily eroded (dissolved) than the surface oxide film. Then, by setting the composition of the etching solution, the conditions for the etching process, etc., the opening width, depth, etc. of the concave portions due to the concave and convex portions formed on the surface can be controlled to a desired size, A snow candy-like protruding portion that protrudes toward the center in the opening width direction can be formed on a part or all of the opening edge.
  • an aqueous hydrochloric acid solution having an acid concentration of 0.1 to 80% by weight, preferably 0.5 to 50% by weight, phosphoric acid
  • halides added for introducing halogen ions include chlorides such as sodium chloride, potassium chloride, magnesium chloride, and aluminum chloride, fluorides such as calcium fluoride, and bromides such as potassium bromide.
  • the halogen ion concentration in the etching solution is usually 0.5 g / liter (g / L) to 300 g / L, preferably 1 g / L to 200 g / L, preferably 0.5 g. If it is less than / L, the effect of halogen ions is small, so that there is a problem that a concave portion having a snow ridge-like protrusion is not formed at the opening edge, and if it exceeds 300 g / L, the surface of the aluminum-shaped body Since the dissolution reaction proceeds rapidly during the processing (etching processing), there arises a problem that it becomes difficult to control the concave portion.
  • an etching solution for forming a desired concave portion on the surface of the aluminum-shaped body may be an aqueous solution or water of a relatively strong oxidizing power such as nitric acid or concentrated sulfuric acid having a concentration exceeding 80% by weight.
  • aqueous solution of an alkali such as sodium oxide or potassium hydroxide is not suitable.
  • An acid aqueous solution having a relatively strong oxidizing power has a film forming ability with respect to an aluminum alloy. On the contrary, a strong oxide film is formed on the surface of the aluminum shaped body, and it becomes difficult to dissolve the oxide film by halogen ions.
  • the dissolution mechanism of an aqueous alkali solution such as sodium hydroxide or potassium hydroxide is the entire surface dissolution type, and the tendency does not change even when halogen ions are added, and the desired shape and size are obtained. It becomes difficult to form the concave portion.
  • the processing conditions for etching the surface of the aluminum alloy material using the above etching solution are required for the type of etching solution used, the acid concentration, the halogen ion concentration, etc., and the aluminum shape.
  • the bath temperature is usually 20 to 80 ° C. for a hydrochloric acid aqueous solution and the immersion time is 1 to 30 minutes, and the bath temperature is 30 to 80 ° C. for a phosphoric acid aqueous solution.
  • the bath temperature is preferably 50 to 80 ° C. and the immersion time is 1 to 3 minutes. The higher the acid concentration and bath temperature of the etching solution to be used, the more effective the etching process becomes and the shorter the processing time is possible.
  • the dissolution reaction proceeds rapidly, making it difficult to control the opening width and depth of the concave portion.
  • the immersion time if the opening time is less than 1 minute, it is difficult to control the opening width and depth of the concave portion, and conversely, if the immersion time exceeds 30 minutes, the productivity is lowered.
  • the surface of the aluminum alloy material before the etching treatment is degreased, surface-adjusted, surface
  • a pretreatment consisting of an acid treatment with an acid aqueous solution and / or an alkali treatment with an alkali solution may be performed.
  • examples of the acid aqueous solution used for this pretreatment include those prepared with commercially available acid degreasing agents, mineral acids such as sulfuric acid, nitric acid, hydrofluoric acid, and phosphoric acid, organic acids such as acetic acid and citric acid, and the like.
  • acid reagents such as a mixed acid obtained by mixing acid
  • alkaline aqueous solution for example, what was prepared with a commercially available alkaline degreasing agent, caustic soda, etc.
  • alkali reagent, or what was prepared by mixing these things etc. can be used.
  • the operation method and treatment conditions of the pretreatment conventionally performed using this type of acid aqueous solution or alkali aqueous solution and For example, it can be performed by a method such as an immersion method or a spray method.
  • the aluminum alloy material that has been subjected to pretreatment and etching treatment is subjected to drying treatment as necessary.
  • This drying treatment may be natural drying that is allowed to stand at room temperature, or may be air blow, dryer, oven, etc. Forced drying may be used.
  • the surface of the aluminum shaped body obtained by the above etching treatment or by the pretreatment and the etching treatment has uneven portions formed by the etching treatment, and the surface has a 60 degree surface glossiness (digital deflection angle manufactured by Suga Test Instruments Co., Ltd.).
  • the measurement with a gloss meter is preferably 60 or less.
  • the surface of the aluminum shaped body obtained by the above etching treatment or by the pretreatment and the etching treatment is observed with a SEM or an optical microscope at a magnification of 1000 times, and the obtained cross-sectional observation photograph is preferably an aluminum shape.
  • the surface area of the body is preferably 1.2 times or more and 10 times or less the surface area of the aluminum alloy material before forming the irregularities by etching treatment.
  • the adhesive does not sufficiently enter the concave portion of the aluminum shape body when the adhesive is applied, and the aluminum shape body and the adhesive layer Adequate adhesion between the two cannot be obtained.
  • a metal or resin adherend is bonded to the aluminum-shaped body obtained as described above via an adhesive layer.
  • the aluminum body Before bonding the adherend to the body, the aluminum body may be pretreated.
  • an acid solution and / or alkali solution containing a silicon compound or a commercially available chromium-free treatment agent may be used.
  • the acid solution and / or alkali solution containing such a silicon compound include an acid solution containing colloidal silica and an alkali solution containing a silicate such as sodium metasilicate.
  • commercially available chromium-free treatment agents include Alsurf and Surfcoat manufactured by Nippon Paint, and Palcoat manufactured by Nippon Parkerizing.
  • an adhesive is applied to the aluminum shape body and / or the adherend, and this coating is applied.
  • the aluminum shape body and the object to be bonded are preferably brought into close contact with each other with pressure therebetween to solidify the adhesive, but the adhesive can be efficiently introduced into the concave portion of the aluminum shape body.
  • an appropriate type of adhesive is selected according to the material of the adherend used, or on the adherend side.
  • a concave portion similar to that in the case of the aluminum shape body may be formed, and the concave portion and the fitting portion formed in the adhesive layer may be locked.
  • the method for applying the adhesive may be a pre-coating method such as a roll coating method, a spray coating method, a dipping method, a brush coating, a roller coating, or a post coating method.
  • coating an adhesive agent before solidifying, the target metal or resin-made to-be-adhered body is joined.
  • a drying method corresponding to the type of the adhesive may be employed. For example, room temperature drying or baking drying is performed using an air blower, a dryer, an oven, or the like. be able to.
  • the target aluminum adhesive composite material is manufactured.
  • a particularly preferable aluminum-adhesive composite material is an aluminum-adhesive composite material in which an adherend is bonded to a part of the surface of an aluminum shaped body via an adhesive layer.
  • the adhesive for forming the adhesive layer formed between the aluminum shaped body and the adherend is not particularly limited. Examples include rubber, epoxy, cyanoacryl, vinyl chloride, plastic, and hot melt.
  • the film thickness of the adhesive layer formed between the aluminum shaped body and the adherend is appropriately selected according to the purpose of use of the aluminum adhesive composite, and is usually 5 ⁇ m or more.
  • the thickness is 5 mm or less, preferably 10 ⁇ m or more and 2000 ⁇ m or less. If the thickness is less than 5 ⁇ m, sufficient bonding strength is not exhibited. On the other hand, if the thickness is more than 5 mm, the effect is saturated and the durability does not change.
  • a metal appropriately selected according to the use is used, but as an example of a suitable one, aluminum, iron, Examples thereof include metals such as copper, zinc and magnesium and alloys thereof.
  • the etching treatment of the present invention may be applied to form an aluminum body having a concave portion. If the metal to be bonded via the adhesive layer is other than aluminum, perform etching treatment with acid, alkali solution, blasting, roughening with polishing paper, polishing treatment, cleaning treatment with solvent, surfactant, etc. The surface may be adjusted.
  • thermoplastic resins thermosetting resins, room temperature curable resins, and the like.
  • polypropylene resin polyethylene resin, acrylonitrile / butadiene / styrene copolymer (ABS), polycarbonate resin, polyamide resin, polyarylene sulfide resin such as polyphenylene sulfide (PPS), polyacetal resin, liquid crystalline resin, polyethylene terephthalate ( PET) and polyester resins such as polybutylene terephthalate (PBT), polyoxymethylene resins, polyimide resins, syndiotactic polystyrene resins, and mixtures of two or more of these thermoplastic resins.
  • ABS acrylonitrile / butadiene / styrene copolymer
  • PPS polycarbonate resin
  • polyamide resin polyamide resin
  • polyarylene sulfide resin such as polyphenylene sulfide (PPS)
  • PPS polyacetal resin
  • Is epoxy resin etc. It is, also, as the cold-curable resin and polyester resin.
  • the surface of these resins may be adjusted by performing a cleaning treatment with an acid, an alkali solution, a solvent, a surfactant, or the like, or a roughening or polishing treatment with a blast or polishing paper before bonding.
  • the aluminum adhesive composite material of the present invention has an extremely high bonding strength at the interface between the aluminum shaped body and the adhesive layer (aluminum / adhesive interface), and has excellent durability even when exposed to harsh environments. It can be maintained and can maintain high reliability over a long period of time. Accordingly, the aluminum adhesive composite material of the present invention includes, for example, building interiors and exteriors, various building members such as building outer walls and interiors, road materials, various cabinets, refrigeration, refrigerator car container interiors and exteriors, refrigeration showcases, automotive parts, It can be suitably used for various products in a wide range of fields such as electric / electronic parts, home appliances, and various daily necessities.
  • FIG. 1 is a cross-sectional schematic view for illustrating a concave portion by copying a cross section in the thickness direction of an aluminum shape according to the first embodiment.
  • FIG. 2 is a cross-sectional explanatory view showing a typical example of the shape of the concave portion conceived from FIG.
  • FIG. 3 is a front view and a side view of each test specimen for evaluation (aluminum test piece, copper test piece, or resin test piece) of an aluminum adhesive composite material prepared for a posiTEST test using an aluminum shaped body.
  • FIG. 4 is a cross-sectional explanatory view showing a state in which the test specimen for evaluation is set on the actuator part of the posiTEST test apparatus during the posiTEST test.
  • FIG. 5 is a diagram for explaining a method for observation and evaluation of an aluminum shape body / adhesive layer / metal adherend or an aluminum shape body / adhesive layer / resin adherend in a test specimen for evaluation.
  • Example 1 [Preparation of aluminum shape] Prepare aluminum pieces (aluminum alloy material) with a size of 50 mm x 50 mm from a 1.0 mm thick aluminum alloy (JIS A1050-H24) plate, and first immerse these pieces in 30 wt% nitric acid aqueous solution at room temperature for 5 minutes. After that, rinse thoroughly with ion-exchanged water, then immerse in a 5 wt% sodium hydroxide solution at 50 ° C. for 1 minute, then rinse with water, and further immerse in a 30 wt% nitric acid aqueous solution at room temperature for 3 minutes, followed by a pretreatment. did.
  • an etching solution (chlorine ion concentration: prepared by adding 54 g / L of aluminum chloride hexahydrate (AlCl 3 .6H 2 O) to a 2.5 wt% hydrochloric acid aqueous solution of the aluminum piece after the above pretreatment. 48g / L) is etched for 4 minutes at 66 ° C and then washed with water, further immersed in a 30wt% nitric acid aqueous solution for 3 minutes at room temperature, then washed with water, dried with hot air at 120 ° C for 5 minutes, and boiled water The aluminum shape body for making the evaluation sample of a test and a salt spray test was created.
  • the thickness of an aluminum shape body first Determine the top line (TL) perpendicular to this thickness direction in the longitudinal section and passing through the highest part of the concavo-convex part, and then generally the same as above, perpendicular to the thickness direction of the aluminum shaped body, and Determining the bottom line passing through the deepest part of the concavo-convex part, further drawing a line segment from the top line (TL) in a direction perpendicular to the bottom line (BL), passing through the middle part of this line segment, and , The distance between the gaps between the aluminum shape on the half line (HL) drawn parallel to the top line (TL) [or bottom line (BL)] (d) and the shape and size of the recessed part formed due to the uneven part on the surface of the aluminum shaped body
  • the cross section of the observed region of the aluminum-shaped body is as shown in, for example, the cross-sectional view of FIG. 1, and a typical example of the shape of the concave portion conceived from FIG. 1 is as shown in FIG.
  • a concave portion having a protruding portion protruding in a snow bowl shape from a part of the opening edge toward the center in the opening width direction (shape a: see FIG. 2 (a)), from the entire opening edge toward the center in the opening width direction
  • a concave portion having a protruding portion protruding like a snow ridge shape b: see FIG.
  • the size (opening width and depth) of the concave portion observed in the cross section of the region where the aluminum body was measured and the ratio thereof were as follows: the concave portion having an opening width of 0.1 ⁇ m to 1 ⁇ m per 0.1 mm square. 10 to 100, 1 to 10 concave portions with an opening width of 1 ⁇ m to 10 ⁇ m, 1 to 3 concave portions with an opening width of 11 ⁇ m to 30 ⁇ m, and a depth within a range of 0.1 ⁇ m to 30 ⁇ m. there were.
  • the concave shape having an opening width of 0.1 ⁇ m to 1 ⁇ m per 0.1 mm square is substantially the same as described above. 10 to 50 parts, 1 to 50 concave parts with an opening width of 1 ⁇ m to 10 ⁇ m, 1 to 2 concave parts with an opening width of 11 ⁇ m to 30 ⁇ m, and a depth range of 0.1 ⁇ m to 20 ⁇ m It was in. The size of the concave portion was hardly changed even when the observation place was changed.
  • the case where the opening width is within a range of 0.1 to 30 ⁇ m and the depth is within a range of 0.1 to 30 ⁇ m is good ( ⁇ ), and the case where the opening is not so is bad ( X).
  • the size of the concave portion observed in the following Examples 2 to 17 and Comparative Examples 1 to 8 was also evaluated based on the same criteria.
  • A1100 material of metal adherend to form aluminum adhesive composite consisting of aluminum shape body, adhesive layer and metal adherend is aluminum (JIS A1100) dedicated dolly (made by Defelsco) attached to the posiTEST test. ; Size: 20 mm ⁇ , A1100 dolly).
  • the oxygen-free copper of C1020 of the metal adherend to form an aluminum-adhesive composite composed of an aluminum shape, an adhesive layer, and a metal adherend was processed into the same shape as in the case of the above A1100 dolly.
  • Resin polyphenylene sulfide (PPS) for forming an aluminum-adhesive composite material composed of an aluminum shape, an adhesive layer, and a resin adherend was also processed into the same shape as in the case of the A1100 dolly.
  • the A1100 dolly was pretreated and etched in the same manner as in the case of the aluminum shape.
  • the C1020 dolly was degreased with alcohol after polishing the surface to which the adhesive adhered with # 240 SiC abrasive paper.
  • PPS dolly polyphenylene sulfide dolly
  • the surface to which the adhesive was adhered was polished with # 240 SiC abrasive paper and then degreased with alcohol.
  • the C1020 dolly and PPS dolly produced in this way were used in the posiTEST test in the same manner as the A1100 dolly.
  • test specimen for evaluation jointing of aluminum shape and adherend with adhesive
  • the aluminum shape body 1 obtained above and the evaluation dolly 4 shown in Tables 1 and 2 are mixed into a two-component epoxy rapid-curing adhesive (a product manufactured by Huntsman Advantest Materials Co., Ltd.).
  • Each test piece of wearing composite material (for evaluation test body) was produced.
  • the peel load at the aluminum / adhesive interface of the test specimen for evaluation is 6.3 MPa for the aluminum test piece, 6.4 MPa for the copper test piece, and 6.2 MPa for the resin test piece. there were.
  • the case where the adhesive layer remains on the entire surface of the aluminum-shaped body is good ( ⁇ )
  • ( ⁇ ) and the case of not remaining on one side of the aluminum-shaped body (interfacial peeling) were evaluated as defective ( ⁇ )
  • both were good ( ⁇ ).
  • the following Examples 2 to 17 and Comparative Examples 1 to 8 were also evaluated based on the same criteria.
  • observation line (OL) When a large number of observation lines (OL) extending in the thickness direction toward each other are drawn at intervals of 0.1 ⁇ m, at least one observation line (OL) is composed of an adhesive layer-aluminum shaped body-adhesive layer. There is one or more laminated portions, and the thickness of the aluminum-shaped body portion of this laminated portion is in the range of 0.1 ⁇ m to 30 ⁇ m, one within the range of 1000 observation lines (OL). The case where it exists in the above ratio is considered good ( ⁇ ), and such When the laminated portion was not in the range of 1000 observation lines (OL) and was evaluated as defective (x), the result was good ( ⁇ ) in all cases.
  • the following Examples 2 to 17 and Comparative Examples 1 to 3 were also evaluated based on the same criteria.
  • Example 2 Except that JIS A1100-H14 was used as the aluminum alloy plate from which the aluminum piece was cut out, an aluminum shaped body was prepared in the same manner as in Example 1 above, and the evaluation dolly was prepared with the materials shown in Table 1 above. A test specimen for evaluation was prepared in the same manner as in Example 1, and the posiTEST test and observation evaluation of the laminated portion of the test specimen for evaluation were performed in the same manner as in Example 1. The results are shown in Table 1 together with the results of Example 1.
  • Example 3 Except that JIS A5052-H34 was used as the aluminum alloy plate from which the aluminum piece was cut out, an aluminum shaped body was prepared in the same manner as in Example 1 above, and the evaluation dolly was prepared with the materials shown in Table 1 above.
  • a test specimen for evaluation was prepared in the same manner as in Example 1, and the posiTEST test and observation evaluation of the laminated portion of the test specimen for evaluation were performed in the same manner as in Example 1. The results are shown in Table 1 together with the results of Example 1.
  • Example 4 In the same manner as in Example 1 above, except that an etching solution (chlorine ion concentration: 30 g / L) prepared by adding 50 g / L sodium chloride in a 50 wt% phosphoric acid aqueous solution was used for the etching treatment, an aluminum shape was used.
  • a test specimen for evaluation was prepared in the same manner as in Example 1 except that an evaluation dolly was prepared using the materials shown in Table 1, and the posiTEST test was performed in the same manner as in Example 1 above. And the observation evaluation of the laminated part of the test specimen for evaluation was carried out. The results are shown in Table 1 together with the results of Example 1.
  • Example 5 An aluminum shaped body was obtained in the same manner as in Example 1 except that an etching solution (chlorine ion concentration: 30 g / L) prepared by adding 50 g / L sodium chloride in a 10 wt% sulfuric acid aqueous solution was used for the etching treatment.
  • a test specimen for evaluation was prepared in the same manner as in Example 1 except that an evaluation dolly was prepared using the materials shown in Table 1. Also, in the same manner as in Example 1, the posiTEST test, And observation evaluation of the laminated part of the test body for evaluation was implemented. The results are shown in Table 1 together with the results of Example 1.
  • Example 6 In the same manner as in Example 1 above, except that an etching solution (chlorine ion concentration: 30 g / L) prepared by adding 50 g / L sodium chloride in a 30 wt% oxalic acid aqueous solution was used for the etching treatment, an aluminum shape was used.
  • a test specimen for evaluation was prepared in the same manner as in Example 1 except that an evaluation dolly was prepared using the materials shown in Table 1, and the posiTEST test was performed in the same manner as in Example 1 above. And the observation evaluation of the laminated part of the test specimen for evaluation was carried out. The results are shown in Table 1 together with the results of Example 1.
  • Example 7 Using the same etching solution as in Example 1 (chlorine ion concentration: 48 g / L), an aluminum shaped body was prepared in the same manner as in Example 1 except that it was immersed at 50 ° C. for 10 minutes.
  • the test specimen for evaluation was prepared in the same manner as in Example 1 except that the evaluation dolly was prepared in the same manner as in Example 1 above, and the posiTEST test and the laminated part of the test specimen for evaluation were Observational evaluation was carried out. The results are shown in Table 1 together with the results of Example 1.
  • Example 9 Using the same etching solution as in Example 1 (chlorine ion concentration: 48 g / L), an aluminum shaped body was prepared in the same manner as in Example 1 except that it was immersed for 15 minutes at 40 ° C.
  • the materials shown in Table 1 The test specimen for evaluation was prepared in the same manner as in Example 1 except that the evaluation dolly was prepared in the same manner as in Example 1 above, and the posiTEST test and the laminated part of the test specimen for evaluation were Observational evaluation was carried out. The results are shown in Table 1 together with the results of Example 1.
  • Example 11 Except for using an etching solution (chlorine ion concentration: 54 g / L) prepared by adding 50 g / L sodium chloride (NaCl) in a 2.5 wt% hydrochloric acid aqueous solution, the same as in Example 1 above.
  • the test specimen for evaluation was prepared in the same manner as in Example 1 except that an aluminum shaped body was prepared and a dolly for evaluation was prepared using the materials shown in Table 1, and the same as in Example 1 above.
  • the posiTEST test and the observation evaluation of the laminated portion of the test specimen for evaluation were performed. The results are shown in Table 1 together with the results of Example 1.
  • Example 12 An aluminum shaped body was used in the same manner as in Example 1 except that a 2.5 wt% hydrochloric acid aqueous solution (chlorine ion concentration: 24 g / L) was used as an etching solution and the substrate was immersed in water at 76 ° C. for 10 minutes and then washed with water.
  • a test specimen for evaluation was prepared in the same manner as in Example 1 except that an evaluation dolly was prepared using the materials shown in Table 1. Also, in the same manner as in Example 1, the posiTEST test, And observation evaluation of the laminated part of the test body for evaluation was implemented. The results are shown in Table 1 together with the results of Example 1.
  • Examples 13 to 16 Immerse for 10 minutes at 30 ° C using an etching solution (chlorine ion concentration: 173 g / L) prepared by adding 268 g / L of aluminum chloride hexahydrate (AlCl 3 ⁇ 6H 2 O) in 6 wt% hydrochloric acid solution
  • etching solution chlorine ion concentration: 173 g / L
  • AlCl 3 ⁇ 6H 2 O aluminum chloride hexahydrate
  • Example 17 Using the same etching solution (chlorine ion concentration: 48 g / L) as in Example 1 and dipping for 20 minutes at 40 ° C., an aluminum shaped body was prepared in the same manner as in Example 1 above, and the materials shown in Table 1
  • the test specimen for evaluation was prepared in the same manner as in Example 1 except that the evaluation dolly was prepared in the same manner as in Example 1 above, and the posiTEST test and the laminated part of the test specimen for evaluation were Observational evaluation was carried out. The results are shown in Table 1 together with the results of Example 1.
  • Example 1 Except that JIS A1050-H24 was used as the aluminum alloy plate, the aluminum shape was prepared without performing the etching treatment only by the pretreatment of Example 1, and the evaluation dolly was prepared with the materials shown in Table 2. A test specimen for evaluation was prepared in the same manner as in Example 1, and the posiTEST test and observation evaluation of the laminated portion of the test specimen for evaluation were performed in the same manner as in Example 1. The results are shown in Table 2.
  • Example 2 JIS A5052-H34 was used as an aluminum alloy plate, and after the pretreatment of Example 1, it was immersed in a 2.5 wt% hydrochloric acid aqueous solution at 66 ° C. for 4 minutes and washed with water, and further washed in a 5 wt% sodium hydroxide solution at 50 ° C. Immerse for 5 minutes, wash with water, and then immerse in 30wt% nitric acid at room temperature for 3 minutes, wash with water, and then dry with 120 ° C hot air for 5 minutes to prepare an aluminum shape, and evaluate the materials shown in Table 2
  • the test specimen for evaluation was prepared in the same manner as in Example 1 except that the dolly for the test was prepared. Also, as in the case of Example 1, the posiTEST test and the observation evaluation of the laminated portion of the test specimen for evaluation were performed. Carried out. The results are shown in Table 2.
  • Example 3 JIS A1100-H14 was used as the aluminum alloy plate, and after the pretreatment of Example 1, it was immersed in a 50 wt% phosphoric acid aqueous solution at 66 ° C. for 4 minutes, washed with water, and then dried with hot air at 120 ° C. for 5 minutes.
  • a test specimen for evaluation was prepared in the same manner as in Example 1 except that an aluminum shaped body was prepared and a dolly for evaluation was prepared using the materials shown in Table 2, and as in the case of Example 1 above, The posiTEST test and the observation evaluation of the laminated part of the test specimen for evaluation were carried out. The results are shown in Table 2.
  • Example 4 JIS A1050-H24 was used as the aluminum alloy plate, and after the pretreatment of Example 1, it was immersed in a 10 wt% sulfuric acid aqueous solution at 66 ° C. for 4 minutes, washed with water, and then dried with hot air at 120 ° C. for 5 minutes.
  • a test specimen for evaluation was prepared in the same manner as in Example 1 except that a shaped body was prepared and an evaluation dolly was prepared using the materials shown in Table 2.
  • posiTEST was prepared. The test and the observation evaluation of the laminated part of the test specimen for evaluation were carried out. The results are shown in Table 2.
  • Example 5 JIS A1050-H24 was used as the aluminum alloy plate, and after the pretreatment of Example 1, it was immersed in a 30 wt% oxalic acid aqueous solution at 66 ° C. for 4 minutes, washed with water, and then dried with hot air at 120 ° C. for 5 minutes.
  • a test specimen for evaluation was prepared in the same manner as in Example 1 except that an aluminum shaped body was prepared and a dolly for evaluation was prepared using the materials shown in Table 2, and as in the case of Example 1 above, The posiTEST test and the observation evaluation of the laminated part of the test specimen for evaluation were carried out. The results are shown in Table 2.
  • Example 7 JIS A1050-H24 was used as the aluminum alloy plate, and after the pretreatment of Example 1, it was immersed in an etching solution composed of a 30 wt% nitric acid aqueous solution for 4 minutes at 66 ° C. and washed with water, and then heated with 120 ° C. hot air for 5 minutes. An aluminum specimen was prepared by drying, and an evaluation specimen was prepared in the same manner as in Example 1 except that an evaluation dolly was prepared with the materials shown in Table 2. In addition, in the case of Example 1 above, Similarly, observation evaluation of the laminated part of the test specimen for posiTEST and evaluation was performed. The results are shown in Table 2.
  • Example 8 JIS A1050-H24 was used as the aluminum alloy plate, and air blasting was performed using alumina having an average particle size of 300 ⁇ m. Thereafter, only the pretreatment of Example 1 was performed to prepare an aluminum shaped body, and an evaluation test body was prepared in the same manner as in Example 1 except that an evaluation dolly was prepared using the materials shown in Table 2. As in the case of Example 1, the posiTEST test and the observation evaluation of the laminated portion of the test specimen for evaluation were performed. The results are shown in Table 2.
  • SYMBOLS 1 Aluminum shape body, TL ... Top line, BL ... Bottom line, HL ... Half line, d ... Opening width, OL ... Observation line, 2 ... Adhesive, 3 ... Concave part, 4 ... Dolly, 5 ... Actuator, 6 ... Dolly fixing jig.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Laminated Bodies (AREA)
  • ing And Chemical Polishing (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

L'invention concerne un composite d'aluminium lié qui présente une excellente durabilité, et dans lequel un article en aluminium formé et un article métallique ou résineux à lier sont liés solidaires par le biais d'une couche adhésive, et la résistance de la liaison interfaciale entre l'article en aluminium formé et la couche adhésive est extrêmement élevée. De plus, l'invention concerne un procédé de fabrication du composite en aluminium lié. Ledit composite contient: un article en aluminium formé présentant des ondulations sur une partie ou sur l'ensemble de sa surface; un article métallique ou résineux à lier placé sur la surface de l'article en aluminium formé; et une couche adhésive qui lie l'article en aluminium formé à l'article à lier. Plusieurs sections concaves sont formées sur la surface de l'article en aluminium formé du fait des ondulations, et des sections de fixation de couche adhésive sont formées au niveau de l'entrée de l'adhésif et de son durcissement dans les sections concaves. L'article en aluminium formé et la couche adhésive sont en prise avec les sections concaves et les sections de fixation.
PCT/JP2010/071973 2009-12-11 2010-12-08 Composite d'aluminium lie et son procede de fabrication WO2011071062A1 (fr)

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CN104718070B (zh) * 2012-10-17 2016-10-26 住友电木株式会社 金属树脂复合体和金属树脂复合体的制造方法
WO2015087720A1 (fr) * 2013-12-13 2015-06-18 住友ベークライト株式会社 Corps composite en résine et métal
WO2015087722A1 (fr) * 2013-12-13 2015-06-18 住友ベークライト株式会社 Corps composite métal-résine
JP6398280B2 (ja) * 2014-04-16 2018-10-03 住友ベークライト株式会社 ギア
JP6421906B1 (ja) * 2017-05-08 2018-11-14 日本軽金属株式会社 接合用アルミニウム塗装材及びアルミ樹脂複合材

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